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[ CAS No. 2530-83-8 ] {[proInfo.proName]}

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Chemical Structure| 2530-83-8
Chemical Structure| 2530-83-8
Structure of 2530-83-8 * Storage: {[proInfo.prStorage]}
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Product Details of [ 2530-83-8 ]

CAS No. :2530-83-8 MDL No. :MFCD00005144
Formula : C9H20O5Si Boiling Point : -
Linear Structure Formula :- InChI Key :BPSIOYPQMFLKFR-UHFFFAOYSA-N
M.W : 236.34 Pubchem ID :17317
Synonyms :

Calculated chemistry of [ 2530-83-8 ]

Physicochemical Properties

Num. heavy atoms : 15
Num. arom. heavy atoms : 0
Fraction Csp3 : 1.0
Num. rotatable bonds : 9
Num. H-bond acceptors : 5.0
Num. H-bond donors : 0.0
Molar Refractivity : 56.56
TPSA : 49.45 Ų

Pharmacokinetics

GI absorption : High
BBB permeant : Yes
P-gp substrate : No
CYP1A2 inhibitor : No
CYP2C19 inhibitor : No
CYP2C9 inhibitor : No
CYP2D6 inhibitor : No
CYP3A4 inhibitor : No
Log Kp (skin permeation) : -7.34 cm/s

Lipophilicity

Log Po/w (iLOGP) : 3.26
Log Po/w (XLOGP3) : 0.56
Log Po/w (WLOGP) : 0.67
Log Po/w (MLOGP) : -1.34
Log Po/w (SILICOS-IT) : 0.1
Consensus Log Po/w : 0.65

Druglikeness

Lipinski : 0.0
Ghose : None
Veber : 0.0
Egan : 0.0
Muegge : 0.0
Bioavailability Score : 0.55

Water Solubility

Log S (ESOL) : -1.06
Solubility : 20.4 mg/ml ; 0.0863 mol/l
Class : Very soluble
Log S (Ali) : -1.17
Solubility : 16.0 mg/ml ; 0.0675 mol/l
Class : Very soluble
Log S (SILICOS-IT) : -1.79
Solubility : 3.79 mg/ml ; 0.016 mol/l
Class : Soluble

Medicinal Chemistry

PAINS : 0.0 alert
Brenk : 2.0 alert
Leadlikeness : 2.0
Synthetic accessibility : 4.22

Safety of [ 2530-83-8 ]

Signal Word:Warning Class:N/A
Precautionary Statements:P264-P280-P302+P352-P312-P337+P313-P305+P351+P338-P362+P364-P332+P313 UN#:N/A
Hazard Statements:H313-H315-H319 Packing Group:N/A
GHS Pictogram:

Application In Synthesis of [ 2530-83-8 ]

* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.

  • Downstream synthetic route of [ 2530-83-8 ]

[ 2530-83-8 ] Synthesis Path-Downstream   1~85

  • 1
  • [ 1202-34-2 ]
  • [ 2530-83-8 ]
  • C19H29N3O5Si [ No CAS ]
  • 2
  • [ 15496-36-3 ]
  • [ 2530-83-8 ]
  • C23H37N3O5Si [ No CAS ]
  • 3
  • [ 2530-83-8 ]
  • [ 1539-42-0 ]
  • C21H33N3O5Si [ No CAS ]
  • 4
  • [ 2530-83-8 ]
  • [ 15395-61-6 ]
  • C22H35N3O5Si [ No CAS ]
  • 5
  • [ 2530-83-8 ]
  • [ 18620-02-5 ]
  • C15H24BrO5Si(1-)*Br(1-)*Mg(2+) [ No CAS ]
  • 6
  • [ 122-20-3 ]
  • [ 2530-83-8 ]
  • [ 1026852-18-5 ]
  • 7
  • [ 102-71-6 ]
  • [ 2530-83-8 ]
  • 1-(3-Oxiranylmethoxy-propyl)-2,8,9-trioxa-5-aza-1-sila-bicyclo[3.3.3]undecane [ No CAS ]
  • 8
  • [ 2530-83-8 ]
  • C78H153N7O27Si6 [ No CAS ]
  • C84H161N7O29Si7 [ No CAS ]
  • 9
  • [ 2530-83-8 ]
  • 1-((2-Hydroxy-ethyl)-{2-hydroxy-3-[3-(3,7,10-trimethyl-2,8,9-trioxa-5-aza-1-sila-bicyclo[3.3.3]undec-1-yl)-propoxy]-propyl}-amino)-3-[3-(3,7,10-trimethyl-2,8,9-trioxa-5-aza-1-sila-bicyclo[3.3.3]undec-1-yl)-propoxy]-propan-2-ol [ No CAS ]
  • C38H73N3O13Si3 [ No CAS ]
  • 10
  • [ 2530-83-8 ]
  • C104H203N9O35Si8 [ No CAS ]
  • C110H211N9O37Si9 [ No CAS ]
  • 11
  • [ 2530-83-8 ]
  • 1-(Bis-{2-hydroxy-3-[3-(3,7,10-trimethyl-2,8,9-trioxa-5-aza-1-sila-bicyclo[3.3.3]undec-1-yl)-propoxy]-propyl}-amino)-3-[3-(3,7,10-trimethyl-2,8,9-trioxa-5-aza-1-sila-bicyclo[3.3.3]undec-1-yl)-propoxy]-propan-2-ol [ No CAS ]
  • [ 1026552-21-5 ]
  • 12
  • [ 2530-83-8 ]
  • 1,4-dimethyl-1,4,7-triazacyclononane [ No CAS ]
  • C17H39N3O5Si [ No CAS ]
YieldReaction ConditionsOperation in experiment
In water;pH 4.3 - 9.0;Reactivity (does not react); Example 1: (Comparative) Hydrolysis of GPS in water is catalysed by addition of acid or base, otherwise the rate of reaction is too slow to warrant use in an industrial process (see Table 1). Addition of ethanol or other solvent rapidly decreases the rate of hydrolysis to unacceptable levels. The addition of acetic acid to high ethanol to water ratio solutions, does not increase the rate of silane hydrolysis. Table 1 Mass % Mass % Mass % PH Minutes to Water Ethanol Silane 83% Conversion 99 0 1 Neutral 2200 99 0 1 4.3 68 99 0 1 9.0 381 4 95 1 Neutral >60000 59 40 1 Neutral 49000
With ethanol; water; at 60℃; for 0.5h; Example 1; Preparation (1): Preparation of Nanoparticle Surface Modifier: 6 g of gamma-(2,3-glycidoxy)propyltrimethoxysilane, 27 ml (about 21.879) of ethanol, and 3 ml (3 g) of water (1 part by weight of alkoxysilane compound and 4.14 parts by weight of an alcohol/water solution, weight ratio of alcohol/water=88:12) were added into a 100 ml beaker. The beaker was sealed with aluminum foil at the top, and was then heated on a hot plate at 60 C. for 30 minutes with stirring. The reaction mixture was allowed to cool off and was then collected in a capped bottle.
With gadolinium(III) trifluoromethanesulfonate; In ethanol-d6; water-d2;Conversion of starting material; Example 5: Effect of Lanthanide Series Catalyst on Hydrolysis. Deuterated water (d2-water), deuterated ethanol and a series of lanthanide catalysts were mixed together according to the mass ratios in Table 5. A known quantity of [Y-GLYCIDOXYPROPYLTRIMETHOXYSILANE] was added to the solution and the reaction was followed using proton NMR spectroscopy. The time to 83% conversion was between 25 minutes and 272 minutes. All the lanthanide (III) (trifluoromethanesulfonate) 3 catalysts were active in hydrolysing [Y-GLYCIDOXYPROPYLTRIMETHOXYSILANE.] Table 5 Catalyst Mol ratio Mol ratio Mol ratio Concentration Mass %. Mass % Mass % Mass % Minutes to Water Silane catalyst silane Water Solvent Silane Catalyst 83% / g dm-3 Conversion LaTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 272 PrTFMS 10 0.2 0.01 8.60 4.1 89. 8 0.96 0.12 58 NdTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 63 SmTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 59 EuTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 43 GaTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 89 DyTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 61 ErTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 57 TmTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 63 YbTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.13 29 YbTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.13 25 [LA=LANTHANUM,] [PR=PRAESEODYMIUM,] Nd=neodymium, [SM=SAMARIUM,] [EU=EUROPIUM, GA=GADOIMIUM,] Dy=dysprosium, [ER=ERBIUM,] [TM=THULIUM,] Yb=ytterbium [TFMS=TRIFLUROMETHYLSULFONATE]
With erbium(III) triflate; In ethanol-d6; water-d2;Conversion of starting material; Example 5: Effect of Lanthanide Series Catalyst on Hydrolysis. Deuterated water (d2-water), deuterated ethanol and a series of lanthanide catalysts were mixed together according to the mass ratios in Table 5. A known quantity of [Y-GLYCIDOXYPROPYLTRIMETHOXYSILANE] was added to the solution and the reaction was followed using proton NMR spectroscopy. The time to 83% conversion was between 25 minutes and 272 minutes. All the lanthanide (III) (trifluoromethanesulfonate) 3 catalysts were active in hydrolysing [Y-GLYCIDOXYPROPYLTRIMETHOXYSILANE.] Table 5 Catalyst Mol ratio Mol ratio Mol ratio Concentration Mass %. Mass % Mass % Mass % Minutes to Water Silane catalyst silane Water Solvent Silane Catalyst 83% / g dm-3 Conversion LaTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 272 PrTFMS 10 0.2 0.01 8.60 4.1 89. 8 0.96 0.12 58 NdTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 63 SmTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 59 EuTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 43 GaTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 89 DyTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 61 ErTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 57 TmTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 63 YbTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.13 29 YbTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.13 25 [LA=LANTHANUM,] [PR=PRAESEODYMIUM,] Nd=neodymium, [SM=SAMARIUM,] [EU=EUROPIUM, GA=GADOIMIUM,] Dy=dysprosium, [ER=ERBIUM,] [TM=THULIUM,] Yb=ytterbium [TFMS=TRIFLUROMETHYLSULFONATE]
With erbium(III) triflate; In ethanol-d6; water-d2;Conversion of starting material; Example 6: Effect of Lanthanide Series Catalyst on Oligomerisation Deuterated water (d2-water), deuterated ethanol (d6-ethanol) and catalyst were mixed together according to the mass ratios in Table 6. A known quantity of y- glycidoxypropyltrimethoxysilane was added to the solution and the oligomerisation reaction was followed using silicon-29 NMR spectroscopy (measured by the rate of loss of monomeric species). Europium (III) and samarium [(III)] [TRIFLUOROMETHANESULFONATE,, WERE] the least effective oligomerisation catalysts and are the preferred catalysts where it is desired to avoid or to minimise oligomerisation, as, for example, in metal surface treatment processes. Ytterbium and erbium [(III)] tend to promote oligomerisation and hence these catalysts are more suitable for use in crosslinked gel formation processes, such as the generation of solgels, aerogels, xerogels and alcogels. Silicon-29 NMR measurements were performed at higher concentrations of silane and lower concentrations of water. The rate of oligomerisation at 1% mass of the silane (measured by proton NMR) is lower than the rate for 10% mass of silane when catalysed by Eu (III) trifluoromethanesulfonate (Table 6). This may also be the case for oligomerisation reactions catalysed by other metals in the lanthanide series. Table 6 Catalyst Mol ratio Mol ratio Mol ratio Concentration Mass % Mass % Mass % Mass % Half life of Water Silane catalyst Silane Water Solvent Silane Catalyst Silanetriol I g dm-3/mins EuTFMS 5 0. 2 0. 01 94. 20 21. 2 48. 9 10. 00 1. 27 141 EuTFMS 10 0.2 0.01 8.60 4.1 89.9 1.07 0.14 2143 YbTFMS 5 0.2 0.01 94.24 21.2 48.8 10.00 1.31 84 ErTFMS 5 0.2 0.01 94.20 21.2 48.9 10.00 1.30 131 SmTFMS 5 0.2 0.01 94.20 21.2 48.9 10.00 1.26 102 LaTFMS 5 0.2 0. 01 94.20 21. 2 48. 9 10. 00 1. 24 <80
With thulium(III) trifluoromethanesulfonate; In ethanol-d6; water-d2;Conversion of starting material; Example 5: Effect of Lanthanide Series Catalyst on Hydrolysis. Deuterated water (d2-water), deuterated ethanol and a series of lanthanide catalysts were mixed together according to the mass ratios in Table 5. A known quantity of [Y-GLYCIDOXYPROPYLTRIMETHOXYSILANE] was added to the solution and the reaction was followed using proton NMR spectroscopy. The time to 83% conversion was between 25 minutes and 272 minutes. All the lanthanide (III) (trifluoromethanesulfonate) 3 catalysts were active in hydrolysing [Y-GLYCIDOXYPROPYLTRIMETHOXYSILANE.] Table 5 Catalyst Mol ratio Mol ratio Mol ratio Concentration Mass %. Mass % Mass % Mass % Minutes to Water Silane catalyst silane Water Solvent Silane Catalyst 83% / g dm-3 Conversion LaTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 272 PrTFMS 10 0.2 0.01 8.60 4.1 89. 8 0.96 0.12 58 NdTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 63 SmTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 59 EuTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 43 GaTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 89 DyTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 61 ErTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 57 TmTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 63 YbTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.13 29 YbTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.13 25 [LA=LANTHANUM,] [PR=PRAESEODYMIUM,] Nd=neodymium, [SM=SAMARIUM,] [EU=EUROPIUM, GA=GADOIMIUM,] Dy=dysprosium, [ER=ERBIUM,] [TM=THULIUM,] Yb=ytterbium [TFMS=TRIFLUROMETHYLSULFONATE]
With dysprosium(III) trifluoromethanesulfonate; In ethanol-d6; water-d2;Conversion of starting material; Example 5: Effect of Lanthanide Series Catalyst on Hydrolysis. Deuterated water (d2-water), deuterated ethanol and a series of lanthanide catalysts were mixed together according to the mass ratios in Table 5. A known quantity of [Y-GLYCIDOXYPROPYLTRIMETHOXYSILANE] was added to the solution and the reaction was followed using proton NMR spectroscopy. The time to 83% conversion was between 25 minutes and 272 minutes. All the lanthanide (III) (trifluoromethanesulfonate) 3 catalysts were active in hydrolysing [Y-GLYCIDOXYPROPYLTRIMETHOXYSILANE.] Table 5 Catalyst Mol ratio Mol ratio Mol ratio Concentration Mass %. Mass % Mass % Mass % Minutes to Water Silane catalyst silane Water Solvent Silane Catalyst 83% / g dm-3 Conversion LaTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 272 PrTFMS 10 0.2 0.01 8.60 4.1 89. 8 0.96 0.12 58 NdTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 63 SmTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 59 EuTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 43 GaTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 89 DyTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 61 ErTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 57 TmTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 63 YbTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.13 29 YbTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.13 25 [LA=LANTHANUM,] [PR=PRAESEODYMIUM,] Nd=neodymium, [SM=SAMARIUM,] [EU=EUROPIUM, GA=GADOIMIUM,] Dy=dysprosium, [ER=ERBIUM,] [TM=THULIUM,] Yb=ytterbium [TFMS=TRIFLUROMETHYLSULFONATE]
With lanthanum(lll) triflate; In ethanol-d6; water-d2;Conversion of starting material; Example 5: Effect of Lanthanide Series Catalyst on Hydrolysis. Deuterated water (d2-water), deuterated ethanol and a series of lanthanide catalysts were mixed together according to the mass ratios in Table 5. A known quantity of [Y-GLYCIDOXYPROPYLTRIMETHOXYSILANE] was added to the solution and the reaction was followed using proton NMR spectroscopy. The time to 83% conversion was between 25 minutes and 272 minutes. All the lanthanide (III) (trifluoromethanesulfonate) 3 catalysts were active in hydrolysing [Y-GLYCIDOXYPROPYLTRIMETHOXYSILANE.] Table 5 Catalyst Mol ratio Mol ratio Mol ratio Concentration Mass %. Mass % Mass % Mass % Minutes to Water Silane catalyst silane Water Solvent Silane Catalyst 83% / g dm-3 Conversion LaTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 272 PrTFMS 10 0.2 0.01 8.60 4.1 89. 8 0.96 0.12 58 NdTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 63 SmTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 59 EuTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 43 GaTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 89 DyTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 61 ErTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 57 TmTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 63 YbTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.13 29 YbTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.13 25 [LA=LANTHANUM,] [PR=PRAESEODYMIUM,] Nd=neodymium, [SM=SAMARIUM,] [EU=EUROPIUM, GA=GADOIMIUM,] Dy=dysprosium, [ER=ERBIUM,] [TM=THULIUM,] Yb=ytterbium [TFMS=TRIFLUROMETHYLSULFONATE]
With lanthanum(lll) triflate; In ethanol-d6; water-d2;Conversion of starting material; Example 6: Effect of Lanthanide Series Catalyst on Oligomerisation Deuterated water (d2-water), deuterated ethanol (d6-ethanol) and catalyst were mixed together according to the mass ratios in Table 6. A known quantity of y- glycidoxypropyltrimethoxysilane was added to the solution and the oligomerisation reaction was followed using silicon-29 NMR spectroscopy (measured by the rate of loss of monomeric species). Europium (III) and samarium [(III)] [TRIFLUOROMETHANESULFONATE,, WERE] the least effective oligomerisation catalysts and are the preferred catalysts where it is desired to avoid or to minimise oligomerisation, as, for example, in metal surface treatment processes. Ytterbium and erbium [(III)] tend to promote oligomerisation and hence these catalysts are more suitable for use in crosslinked gel formation processes, such as the generation of solgels, aerogels, xerogels and alcogels. Silicon-29 NMR measurements were performed at higher concentrations of silane and lower concentrations of water. The rate of oligomerisation at 1% mass of the silane (measured by proton NMR) is lower than the rate for 10% mass of silane when catalysed by Eu (III) trifluoromethanesulfonate (Table 6). This may also be the case for oligomerisation reactions catalysed by other metals in the lanthanide series. Table 6 Catalyst Mol ratio Mol ratio Mol ratio Concentration Mass % Mass % Mass % Mass % Half life of Water Silane catalyst Silane Water Solvent Silane Catalyst Silanetriol I g dm-3/mins EuTFMS 5 0. 2 0. 01 94. 20 21. 2 48. 9 10. 00 1. 27 141 EuTFMS 10 0.2 0.01 8.60 4.1 89.9 1.07 0.14 2143 YbTFMS 5 0.2 0.01 94.24 21.2 48.8 10.00 1.31 84 ErTFMS 5 0.2 0.01 94.20 21.2 48.9 10.00 1.30 131 SmTFMS 5 0.2 0.01 94.20 21.2 48.9 10.00 1.26 102 LaTFMS 5 0.2 0. 01 94.20 21. 2 48. 9 10. 00 1. 24 <80
With praseodymium(III) trifluoromethanesulfonate; In ethanol-d6; water-d2;Conversion of starting material; Example 5: Effect of Lanthanide Series Catalyst on Hydrolysis. Deuterated water (d2-water), deuterated ethanol and a series of lanthanide catalysts were mixed together according to the mass ratios in Table 5. A known quantity of [Y-GLYCIDOXYPROPYLTRIMETHOXYSILANE] was added to the solution and the reaction was followed using proton NMR spectroscopy. The time to 83% conversion was between 25 minutes and 272 minutes. All the lanthanide (III) (trifluoromethanesulfonate) 3 catalysts were active in hydrolysing [Y-GLYCIDOXYPROPYLTRIMETHOXYSILANE.] Table 5 Catalyst Mol ratio Mol ratio Mol ratio Concentration Mass %. Mass % Mass % Mass % Minutes to Water Silane catalyst silane Water Solvent Silane Catalyst 83% / g dm-3 Conversion LaTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 272 PrTFMS 10 0.2 0.01 8.60 4.1 89. 8 0.96 0.12 58 NdTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 63 SmTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 59 EuTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 43 GaTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 89 DyTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 61 ErTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 57 TmTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 63 YbTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.13 29 YbTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.13 25 [LA=LANTHANUM,] [PR=PRAESEODYMIUM,] Nd=neodymium, [SM=SAMARIUM,] [EU=EUROPIUM, GA=GADOIMIUM,] Dy=dysprosium, [ER=ERBIUM,] [TM=THULIUM,] Yb=ytterbium [TFMS=TRIFLUROMETHYLSULFONATE]
With samarium(III) trifluoromethanesulfonate; In ethanol-d6; water-d2;Conversion of starting material; Example 5: Effect of Lanthanide Series Catalyst on Hydrolysis. Deuterated water (d2-water), deuterated ethanol and a series of lanthanide catalysts were mixed together according to the mass ratios in Table 5. A known quantity of [Y-GLYCIDOXYPROPYLTRIMETHOXYSILANE] was added to the solution and the reaction was followed using proton NMR spectroscopy. The time to 83% conversion was between 25 minutes and 272 minutes. All the lanthanide (III) (trifluoromethanesulfonate) 3 catalysts were active in hydrolysing [Y-GLYCIDOXYPROPYLTRIMETHOXYSILANE.] Table 5 Catalyst Mol ratio Mol ratio Mol ratio Concentration Mass %. Mass % Mass % Mass % Minutes to Water Silane catalyst silane Water Solvent Silane Catalyst 83% / g dm-3 Conversion LaTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 272 PrTFMS 10 0.2 0.01 8.60 4.1 89. 8 0.96 0.12 58 NdTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 63 SmTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 59 EuTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 43 GaTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 89 DyTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 61 ErTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 57 TmTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 63 YbTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.13 29 YbTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.13 25 [LA=LANTHANUM,] [PR=PRAESEODYMIUM,] Nd=neodymium, [SM=SAMARIUM,] [EU=EUROPIUM, GA=GADOIMIUM,] Dy=dysprosium, [ER=ERBIUM,] [TM=THULIUM,] Yb=ytterbium [TFMS=TRIFLUROMETHYLSULFONATE]
With samarium(III) trifluoromethanesulfonate; In ethanol-d6; water-d2;Conversion of starting material; Example 6: Effect of Lanthanide Series Catalyst on Oligomerisation Deuterated water (d2-water), deuterated ethanol (d6-ethanol) and catalyst were mixed together according to the mass ratios in Table 6. A known quantity of y- glycidoxypropyltrimethoxysilane was added to the solution and the oligomerisation reaction was followed using silicon-29 NMR spectroscopy (measured by the rate of loss of monomeric species). Europium (III) and samarium [(III)] [TRIFLUOROMETHANESULFONATE,, WERE] the least effective oligomerisation catalysts and are the preferred catalysts where it is desired to avoid or to minimise oligomerisation, as, for example, in metal surface treatment processes. Ytterbium and erbium [(III)] tend to promote oligomerisation and hence these catalysts are more suitable for use in crosslinked gel formation processes, such as the generation of solgels, aerogels, xerogels and alcogels. Silicon-29 NMR measurements were performed at higher concentrations of silane and lower concentrations of water. The rate of oligomerisation at 1% mass of the silane (measured by proton NMR) is lower than the rate for 10% mass of silane when catalysed by Eu (III) trifluoromethanesulfonate (Table 6). This may also be the case for oligomerisation reactions catalysed by other metals in the lanthanide series. Table 6 Catalyst Mol ratio Mol ratio Mol ratio Concentration Mass % Mass % Mass % Mass % Half life of Water Silane catalyst Silane Water Solvent Silane Catalyst Silanetriol I g dm-3/mins EuTFMS 5 0. 2 0. 01 94. 20 21. 2 48. 9 10. 00 1. 27 141 EuTFMS 10 0.2 0.01 8.60 4.1 89.9 1.07 0.14 2143 YbTFMS 5 0.2 0.01 94.24 21.2 48.8 10.00 1.31 84 ErTFMS 5 0.2 0.01 94.20 21.2 48.9 10.00 1.30 131 SmTFMS 5 0.2 0.01 94.20 21.2 48.9 10.00 1.26 102 LaTFMS 5 0.2 0. 01 94.20 21. 2 48. 9 10. 00 1. 24 <80
With europium(III) trifluoromethanesulfonate; In ethanol-d6; water-d2;Conversion of starting material; Example 5: Effect of Lanthanide Series Catalyst on Hydrolysis. Deuterated water (d2-water), deuterated ethanol and a series of lanthanide catalysts were mixed together according to the mass ratios in Table 5. A known quantity of [Y-GLYCIDOXYPROPYLTRIMETHOXYSILANE] was added to the solution and the reaction was followed using proton NMR spectroscopy. The time to 83% conversion was between 25 minutes and 272 minutes. All the lanthanide (III) (trifluoromethanesulfonate) 3 catalysts were active in hydrolysing [Y-GLYCIDOXYPROPYLTRIMETHOXYSILANE.] Table 5 Catalyst Mol ratio Mol ratio Mol ratio Concentration Mass %. Mass % Mass % Mass % Minutes to Water Silane catalyst silane Water Solvent Silane Catalyst 83% / g dm-3 Conversion LaTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 272 PrTFMS 10 0.2 0.01 8.60 4.1 89. 8 0.96 0.12 58 NdTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 63 SmTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 59 EuTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 43 GaTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 89 DyTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 61 ErTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 57 TmTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 63 YbTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.13 29 YbTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.13 25 [LA=LANTHANUM,] [PR=PRAESEODYMIUM,] Nd=neodymium, [SM=SAMARIUM,] [EU=EUROPIUM, GA=GADOIMIUM,] Dy=dysprosium, [ER=ERBIUM,] [TM=THULIUM,] Yb=ytterbium [TFMS=TRIFLUROMETHYLSULFONATE]
With europium(III) trifluoromethanesulfonate; In ethanol-d6; water-d2;Conversion of starting material; Example 6: Effect of Lanthanide Series Catalyst on Oligomerisation Deuterated water (d2-water), deuterated ethanol (d6-ethanol) and catalyst were mixed together according to the mass ratios in Table 6. A known quantity of y- glycidoxypropyltrimethoxysilane was added to the solution and the oligomerisation reaction was followed using silicon-29 NMR spectroscopy (measured by the rate of loss of monomeric species). Europium (III) and samarium [(III)] [TRIFLUOROMETHANESULFONATE,, WERE] the least effective oligomerisation catalysts and are the preferred catalysts where it is desired to avoid or to minimise oligomerisation, as, for example, in metal surface treatment processes. Ytterbium and erbium [(III)] tend to promote oligomerisation and hence these catalysts are more suitable for use in crosslinked gel formation processes, such as the generation of solgels, aerogels, xerogels and alcogels. Silicon-29 NMR measurements were performed at higher concentrations of silane and lower concentrations of water. The rate of oligomerisation at 1% mass of the silane (measured by proton NMR) is lower than the rate for 10% mass of silane when catalysed by Eu (III) trifluoromethanesulfonate (Table 6). This may also be the case for oligomerisation reactions catalysed by other metals in the lanthanide series. Table 6 Catalyst Mol ratio Mol ratio Mol ratio Concentration Mass % Mass % Mass % Mass % Half life of Water Silane catalyst Silane Water Solvent Silane Catalyst Silanetriol I g dm-3/mins EuTFMS 5 0. 2 0. 01 94. 20 21. 2 48. 9 10. 00 1. 27 141 EuTFMS 10 0.2 0.01 8.60 4.1 89.9 1.07 0.14 2143 YbTFMS 5 0.2 0.01 94.24 21.2 48.8 10.00 1.31 84 ErTFMS 5 0.2 0.01 94.20 21.2 48.9 10.00 1.30 131 SmTFMS 5 0.2 0.01 94.20 21.2 48.9 10.00 1.26 102 LaTFMS 5 0.2 0. 01 94.20 21. 2 48. 9 10. 00 1. 24 <80
With europium(III) trifluoromethanesulfonate; In ethanol-d6; water-d2; at 25 - 90℃; for 1h;Conversion of starting material; Example 8 Effect of La Series Catalyst on metal Surface Condensation Deuterated water (d2-water), deuterated ethanol (d6-ethanol), europium (III) trifluoromethanesulfonate) 3 (catalyst) and GPS were mixed together according to the mass ratio of 30.1 : 695: 1: 7.9 respectively. The solution was hydrolysed at [25C] for one hour. The hydrolysed silane solution was dripped onto degreased, grit- blasted stainless steel and the surface was air dried to remove volatile solvent leaving a thin coating (0.1 to 10 microns) of monomeric hydrolysed silane. The condensation reaction was followed by diffuse reflectance infrared spectroscopy at temperatures in the range [OF 30C] to [90C.] For comparative purposes, a condensation reaction according to a current state of the art silane treatment system was carried out. The hydrolysis of GPS in water and ethanol (mass ratio of 1: 2: 18) was catalysed by the addition of acid (pH of 3.7). The solution'was hydrolysed for one hour at [25C] before applying onto degreased, grit-blasted stainless steel. The residual solvent was evaporated from the surface by air drying. The condensation reaction was followed by diffuse reflectance infrared spectroscopy at temperatures in the range [OF 30C] to [90C.] The results are shown in Table 8. The disappearance of the hydroxyl band in the infrared spectroscopy (band centred around 3375 [CM-L)] gave a measure at which the monomeric hydroxyl silane condensed to form a highly crosslinked siloxane film. The kinetic curves are complex and are not first, second or simple n order rate processes. A measure of the reaction rate, in Table 8, is given by the peak ratio of the OH band to CH band (centered at [2800CM~L)] at a time interval of 50 minutes. At equivalent temperatures, the condensation reaction has progressed to a greater extent for the europium (III) trifluoromethanesulphonate catalysed system relative to the acid catalysed system. Near the end of the condensation reaction the OH content forms an equilibrium, as there appears to be no further change with time. This suggests that the condensation process is limited either by diffusion processes or by the chemistry of the structure (eg. steric hindrance). However, at equivalent temperatures, the europium (III) trifluoromethane sulphonate catalysed system contains less OH than the acid catalysed system suggesting that the lanthanide salt catalyses the condensation process to a greater extent than the acid catalysed system. A comparison of the rare earth metal catalysed reaction process with that of the current state of the art methodology therefore indicates that the lanthanide catalysts not only increases the rate at which the silane condenses to a highly crosslinked film but also it increases the extent of the reaction. Table 8 Catalyst Temperature C Peak ratio at Peak ratio at 50 mins measurement end EuTFMS 30 2.03 1.75 EuTFMS 40 1.89 1.68 EuTFMS 50 1.81 1.31 EuTFMS 60 1.52 0.91 EuTFMS 70 1.04 0.71 EuTFMS 80 1. 26 1.22 EuTFMS 90 0.81 0.82 Acid catalyst 30 2.53 1.99 Acid catalyst 40 2.24 1.96 Acid catalyst 50 2.01 1.84 Acid catalyst 70 1.69 1.61 Acid catalyst 80 1. 51 1.44 Acid catalyst 90 1.53 1.43
With europium(III) trifluoromethanesulfonate; In ethanol-d6; water-d2; at 20 - 35℃;Conversion of starting material; Example 7: Effect of Europium Salt and Temperature on Silane Hydrolysis Unless otherwise specified, deuterated water (d2-water), deuterated ethanol (d6-ethanol) and catalyst were mixed together according to the mass ratios in Table 7. A known quantity of y-glycidoxypropyltrimethoxysilane was added to the solution and the hydrolysis reaction was followed using proton NMR spectroscopy (measured by the rate of formation of methanol). The time to 83% conversion typically took between 11 minutes and more than 2500 minutes. Europium perchlorate was the best catalyst for silane hydrolysis. The activation energy for GPS hydrolysis was calculated to be 57 kJ per mole. Using the same mol ratio of reactants and solvents, there is found to be little difference between the hydrolysis rates in protic solvents (sample [EUTFMS] (1), Table 7) and in deuterated solvents. Table 7 Catalyst Concentration Mass % Mass % Mass % Mass % Temperature Minutes to Silane Water Solvent Silane catalyst/C 83% /g dm-3 Conversion EuTFMS 8. 60 4. 06 94. 86 0. 96 0. 12 30 44 EuTFMS 8.60 4.06 94.86 0.96 0.12 35 21 EuTFMS 8.60 4.06 94.86 0.96 0.12 20 116 EuOxalate. XH20 8.60 4.06 94.87 0.96 0.12 25 >5000 Eu perchlorate 8.55 4.04 94.92 0.95 0.09 25 11 Eu nitrate 8.60 4.06 94.89 0.96 0.09 25 2574 pentahydrate EuTFMS (1) # 7.64 3.64 95.28 0.96 0.12 25 44 # solvent was protonated ethanol and water (ie. non-deuterated)
With europium(III) oxalate; In ethanol-d6; water-d2;Conversion of starting material; Example 7: Effect of Europium Salt and Temperature on Silane Hydrolysis Unless otherwise specified, deuterated water (d2-water), deuterated ethanol (d6-ethanol) and catalyst were mixed together according to the mass ratios in Table 7. A known quantity of y-glycidoxypropyltrimethoxysilane was added to the solution and the hydrolysis reaction was followed using proton NMR spectroscopy (measured by the rate of formation of methanol). The time to 83% conversion typically took between 11 minutes and more than 2500 minutes. Europium perchlorate was the best catalyst for silane hydrolysis. The activation energy for GPS hydrolysis was calculated to be 57 kJ per mole. Using the same mol ratio of reactants and solvents, there is found to be little difference between the hydrolysis rates in protic solvents (sample [EUTFMS] (1), Table 7) and in deuterated solvents. Table 7 Catalyst Concentration Mass % Mass % Mass % Mass % Temperature Minutes to Silane Water Solvent Silane catalyst/C 83% /g dm-3 Conversion EuTFMS 8. 60 4. 06 94. 86 0. 96 0. 12 30 44 EuTFMS 8.60 4.06 94.86 0.96 0.12 35 21 EuTFMS 8.60 4.06 94.86 0.96 0.12 20 116 EuOxalate. XH20 8.60 4.06 94.87 0.96 0.12 25 >5000 Eu perchlorate 8.55 4.04 94.92 0.95 0.09 25 11 Eu nitrate 8.60 4.06 94.89 0.96 0.09 25 2574 pentahydrate EuTFMS (1) # 7.64 3.64 95.28 0.96 0.12 25 44 # solvent was protonated ethanol and water (ie. non-deuterated)
With europium(III) perchlorate; In ethanol-d6; water-d2;Conversion of starting material; Example 7: Effect of Europium Salt and Temperature on Silane Hydrolysis Unless otherwise specified, deuterated water (d2-water), deuterated ethanol (d6-ethanol) and catalyst were mixed together according to the mass ratios in Table 7. A known quantity of y-glycidoxypropyltrimethoxysilane was added to the solution and the hydrolysis reaction was followed using proton NMR spectroscopy (measured by the rate of formation of methanol). The time to 83% conversion typically took between 11 minutes and more than 2500 minutes. Europium perchlorate was the best catalyst for silane hydrolysis. The activation energy for GPS hydrolysis was calculated to be 57 kJ per mole. Using the same mol ratio of reactants and solvents, there is found to be little difference between the hydrolysis rates in protic solvents (sample [EUTFMS] (1), Table 7) and in deuterated solvents. Table 7 Catalyst Concentration Mass % Mass % Mass % Mass % Temperature Minutes to Silane Water Solvent Silane catalyst/C 83% /g dm-3 Conversion EuTFMS 8. 60 4. 06 94. 86 0. 96 0. 12 30 44 EuTFMS 8.60 4.06 94.86 0.96 0.12 35 21 EuTFMS 8.60 4.06 94.86 0.96 0.12 20 116 EuOxalate. XH20 8.60 4.06 94.87 0.96 0.12 25 >5000 Eu perchlorate 8.55 4.04 94.92 0.95 0.09 25 11 Eu nitrate 8.60 4.06 94.89 0.96 0.09 25 2574 pentahydrate EuTFMS (1) # 7.64 3.64 95.28 0.96 0.12 25 44 # solvent was protonated ethanol and water (ie. non-deuterated)
With europium(III) nitrate; In ethanol-d6; water-d2;Conversion of starting material; Example 7: Effect of Europium Salt and Temperature on Silane Hydrolysis Unless otherwise specified, deuterated water (d2-water), deuterated ethanol (d6-ethanol) and catalyst were mixed together according to the mass ratios in Table 7. A known quantity of y-glycidoxypropyltrimethoxysilane was added to the solution and the hydrolysis reaction was followed using proton NMR spectroscopy (measured by the rate of formation of methanol). The time to 83% conversion typically took between 11 minutes and more than 2500 minutes. Europium perchlorate was the best catalyst for silane hydrolysis. The activation energy for GPS hydrolysis was calculated to be 57 kJ per mole. Using the same mol ratio of reactants and solvents, there is found to be little difference between the hydrolysis rates in protic solvents (sample [EUTFMS] (1), Table 7) and in deuterated solvents. Table 7 Catalyst Concentration Mass % Mass % Mass % Mass % Temperature Minutes to Silane Water Solvent Silane catalyst/C 83% /g dm-3 Conversion EuTFMS 8. 60 4. 06 94. 86 0. 96 0. 12 30 44 EuTFMS 8.60 4.06 94.86 0.96 0.12 35 21 EuTFMS 8.60 4.06 94.86 0.96 0.12 20 116 EuOxalate. XH20 8.60 4.06 94.87 0.96 0.12 25 >5000 Eu perchlorate 8.55 4.04 94.92 0.95 0.09 25 11 Eu nitrate 8.60 4.06 94.89 0.96 0.09 25 2574 pentahydrate EuTFMS (1) # 7.64 3.64 95.28 0.96 0.12 25 44 # solvent was protonated ethanol and water (ie. non-deuterated)
With neodymium(III) trifluoromethanesufonate; In ethanol-d6; water-d2;Conversion of starting material; Example 5: Effect of Lanthanide Series Catalyst on Hydrolysis. Deuterated water (d2-water), deuterated ethanol and a series of lanthanide catalysts were mixed together according to the mass ratios in Table 5. A known quantity of [Y-GLYCIDOXYPROPYLTRIMETHOXYSILANE] was added to the solution and the reaction was followed using proton NMR spectroscopy. The time to 83% conversion was between 25 minutes and 272 minutes. All the lanthanide (III) (trifluoromethanesulfonate) 3 catalysts were active in hydrolysing [Y-GLYCIDOXYPROPYLTRIMETHOXYSILANE.] Table 5 Catalyst Mol ratio Mol ratio Mol ratio Concentration Mass %. Mass % Mass % Mass % Minutes to Water Silane catalyst silane Water Solvent Silane Catalyst 83% / g dm-3 Conversion LaTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 272 PrTFMS 10 0.2 0.01 8.60 4.1 89. 8 0.96 0.12 58 NdTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 63 SmTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 59 EuTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 43 GaTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 89 DyTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 61 ErTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 57 TmTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 63 YbTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.13 29 YbTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.13 25 [LA=LANTHANUM,] [PR=PRAESEODYMIUM,] Nd=neodymium, [SM=SAMARIUM,] [EU=EUROPIUM, GA=GADOIMIUM,] Dy=dysprosium, [ER=ERBIUM,] [TM=THULIUM,] Yb=ytterbium [TFMS=TRIFLUROMETHYLSULFONATE]
With ytterbium(III) triflate; In d(4)-methanol; water-d2;Conversion of starting material; Example 4: Effect of silane on Yb [(OTF) 3] catalysed system Deuterated water (d2-water), deuterated methanol and ytterbium trifluoromethanesulfonate were mixed together according to the mass ratios in Table 4. A'known quantity of silane was added to the solution and the reaction was followed using proton NMR spectroscopy. The time to 83% conversion was between 6 minutes and 425 minutes. All the silanes underwent hydrolysis; however, vinyl trimethoxysilane and [3-] trimethoxysilylpropylacrylate reacted rapidly within 15 minutes. The 3- [AMINOPROPYLTRIETHOXYSILANE] rapidly crosslinked within an hour to form a gel like material. The kinetics of this reaction could not be followed by proton NMR spectroscopy. This example shows that the non hydrolysable group attached to the silicon atom has a great effect on the reactivity of the silane. However, for surface coating solutions it will generally be desired that the side chain should have certain specific properties and for this reason the coatings industry tends to be directed towards the use of particular silanes. Table 4 Mol Mol Mol Concn. Mass % Mass % Mass Mass % Minutes to Silane ratio ratio ratio % Water silane Catalyst Silane Water Solvent Silane catalyst 83% Conversion /g dm-3 Vinyl trimethoxy silane 10 0. 2 0. 01 8. 6 6. 4 92. 4 0. 95 0. 20 11. 3 3- (trimethoxysilyl) propyl 10 0.2 0.01 8.6 4.1 94.8 0.96 0.13 6.1 acrylate GPS 10 0.2 0.01 8.6 4.1 94.9 0.96 0.13 28.8 Triethoxyvinylsilane 10 0.2 0.01 8.6 5.0 93.8 0.96 0.16 25.4 Triethoxysilylpropylethylen 10 0.2 0.01 8.6 4.3 94.6 0.96 0.13 31.3 diamine dc 3-10 0.2 0.01 8.6 4.3 94.6 0.96 0.13 Gel aminopropyltriethoxysilane dc 3- (triethoxysilyl) propyl 10 0.2 0.01 8.6 3.9 95.0 0.96 0.12 425.5 isocyanate GPS (SipB) 10 0.2 0.01 8.6 4.1 94.9 0. 96 0.13 16.4
With ytterbium(III) triflate; In tetrahydrofuran-d8; water-d2;Conversion of starting material; Example 3: Effect of solvent on Yb (OTf) 3 catalysed system Deuterated water (d2-water), deuterated solvent and ytterbium trifluoromethanesulfonate were mixed together according to the mass ratios in Table 3. A known quantity [OF Y-GLYCIDOXYPROPYLTRIMETHOXYSILANE] was added to the solution and the reaction was followed using proton NMR spectroscopy. The time taken to 83% conversion was between 23 minutes and 182752 minutes. Although the reaction was shown to take place in THF and dioxane, for industrial purposes, high concentrations of THF and dioxane are impracticable. It should be noted that the reaction proceeds faster in a more polar solvent and the best results are in protic solvents such as ethanol and methanol. Table 3 Mol ratio Mol ratio Mol ratio Concentration Solvent Mass Mass Mass Mass % Minutes to water silane catalyst silane % % % 83% /g dm-3 Water Solvent Silane Catalyst Conversion 10 0. 1 0. 01 12. 9 EtOD 12. 0 86.3 1.4 0. 37 47 10 0.2 0.01 8.6 EtOD 4.1 94.9 1.0 0.13 29 10 0.1 0.01 12.9 MeOD 12.0 86.3 1.4 0.37 58 10 0.2 0.01 8.6 MeOD 4.1 94.9 1.0 0.13 23 10 0.1 0.01 12.9 THF 10.9 87.4 1.3 0.34 416 10 0.2 0.01 8.6 THF 3.7 95.3 0.9 0.11 2682 10 0.1 0.01 12.9 D6-Acetone 12.2 86.0 1.4 0.38 173 10 0.2 0.01 8.6 D6-Acetone 4.1 94.8 1.0 0.13 267 10 0.1 0.01 12.9 ACN 12.5 85.6 1.5 0.39 142 10 0.2 0.01 8.6 ACN 4.3 94.6 1.0 0.13 124 10 0.1 0.01 12.9 dioxane 9.7 88.9 1.1 0.30 2084 10 0.2 0.01 8.6 dioxane 3. 2 95.9 0.8 0. 10 18272
With ytterbium(III) triflate; In deuteromethanol; water-d2;Conversion of starting material; Example 3: Effect of solvent on Yb (OTf) 3 catalysed system Deuterated water (d2-water), deuterated solvent and ytterbium trifluoromethanesulfonate were mixed together according to the mass ratios in Table 3. A known quantity [OF Y-GLYCIDOXYPROPYLTRIMETHOXYSILANE] was added to the solution and the reaction was followed using proton NMR spectroscopy. The time taken to 83% conversion was between 23 minutes and 182752 minutes. Although the reaction was shown to take place in THF and dioxane, for industrial purposes, high concentrations of THF and dioxane are impracticable. It should be noted that the reaction proceeds faster in a more polar solvent and the best results are in protic solvents such as ethanol and methanol. Table 3 Mol ratio Mol ratio Mol ratio Concentration Solvent Mass Mass Mass Mass % Minutes to water silane catalyst silane % % % 83% /g dm-3 Water Solvent Silane Catalyst Conversion 10 0. 1 0. 01 12. 9 EtOD 12. 0 86.3 1.4 0. 37 47 10 0.2 0.01 8.6 EtOD 4.1 94.9 1.0 0.13 29 10 0.1 0.01 12.9 MeOD 12.0 86.3 1.4 0.37 58 10 0.2 0.01 8.6 MeOD 4.1 94.9 1.0 0.13 23 10 0.1 0.01 12.9 THF 10.9 87.4 1.3 0.34 416 10 0.2 0.01 8.6 THF 3.7 95.3 0.9 0.11 2682 10 0.1 0.01 12.9 D6-Acetone 12.2 86.0 1.4 0.38 173 10 0.2 0.01 8.6 D6-Acetone 4.1 94.8 1.0 0.13 267 10 0.1 0.01 12.9 ACN 12.5 85.6 1.5 0.39 142 10 0.2 0.01 8.6 ACN 4.3 94.6 1.0 0.13 124 10 0.1 0.01 12.9 dioxane 9.7 88.9 1.1 0.30 2084 10 0.2 0.01 8.6 dioxane 3. 2 95.9 0.8 0. 10 18272
With ytterbium(III) triflate; In 1,4-dioxane-d8; water-d2;Conversion of starting material; Example 3: Effect of solvent on Yb (OTf) 3 catalysed system Deuterated water (d2-water), deuterated solvent and ytterbium trifluoromethanesulfonate were mixed together according to the mass ratios in Table 3. A known quantity [OF Y-GLYCIDOXYPROPYLTRIMETHOXYSILANE] was added to the solution and the reaction was followed using proton NMR spectroscopy. The time taken to 83% conversion was between 23 minutes and 182752 minutes. Although the reaction was shown to take place in THF and dioxane, for industrial purposes, high concentrations of THF and dioxane are impracticable. It should be noted that the reaction proceeds faster in a more polar solvent and the best results are in protic solvents such as ethanol and methanol. Table 3 Mol ratio Mol ratio Mol ratio Concentration Solvent Mass Mass Mass Mass % Minutes to water silane catalyst silane % % % 83% /g dm-3 Water Solvent Silane Catalyst Conversion 10 0. 1 0. 01 12. 9 EtOD 12. 0 86.3 1.4 0. 37 47 10 0.2 0.01 8.6 EtOD 4.1 94.9 1.0 0.13 29 10 0.1 0.01 12.9 MeOD 12.0 86.3 1.4 0.37 58 10 0.2 0.01 8.6 MeOD 4.1 94.9 1.0 0.13 23 10 0.1 0.01 12.9 THF 10.9 87.4 1.3 0.34 416 10 0.2 0.01 8.6 THF 3.7 95.3 0.9 0.11 2682 10 0.1 0.01 12.9 D6-Acetone 12.2 86.0 1.4 0.38 173 10 0.2 0.01 8.6 D6-Acetone 4.1 94.8 1.0 0.13 267 10 0.1 0.01 12.9 ACN 12.5 85.6 1.5 0.39 142 10 0.2 0.01 8.6 ACN 4.3 94.6 1.0 0.13 124 10 0.1 0.01 12.9 dioxane 9.7 88.9 1.1 0.30 2084 10 0.2 0.01 8.6 dioxane 3. 2 95.9 0.8 0. 10 18272
With ytterbium(III) triflate; In [D3]acetonitrile; water-d2;Conversion of starting material; Example 3: Effect of solvent on Yb (OTf) 3 catalysed system Deuterated water (d2-water), deuterated solvent and ytterbium trifluoromethanesulfonate were mixed together according to the mass ratios in Table 3. A known quantity [OF Y-GLYCIDOXYPROPYLTRIMETHOXYSILANE] was added to the solution and the reaction was followed using proton NMR spectroscopy. The time taken to 83% conversion was between 23 minutes and 182752 minutes. Although the reaction was shown to take place in THF and dioxane, for industrial purposes, high concentrations of THF and dioxane are impracticable. It should be noted that the reaction proceeds faster in a more polar solvent and the best results are in protic solvents such as ethanol and methanol. Table 3 Mol ratio Mol ratio Mol ratio Concentration Solvent Mass Mass Mass Mass % Minutes to water silane catalyst silane % % % 83% /g dm-3 Water Solvent Silane Catalyst Conversion 10 0. 1 0. 01 12. 9 EtOD 12. 0 86.3 1.4 0. 37 47 10 0.2 0.01 8.6 EtOD 4.1 94.9 1.0 0.13 29 10 0.1 0.01 12.9 MeOD 12.0 86.3 1.4 0.37 58 10 0.2 0.01 8.6 MeOD 4.1 94.9 1.0 0.13 23 10 0.1 0.01 12.9 THF 10.9 87.4 1.3 0.34 416 10 0.2 0.01 8.6 THF 3.7 95.3 0.9 0.11 2682 10 0.1 0.01 12.9 D6-Acetone 12.2 86.0 1.4 0.38 173 10 0.2 0.01 8.6 D6-Acetone 4.1 94.8 1.0 0.13 267 10 0.1 0.01 12.9 ACN 12.5 85.6 1.5 0.39 142 10 0.2 0.01 8.6 ACN 4.3 94.6 1.0 0.13 124 10 0.1 0.01 12.9 dioxane 9.7 88.9 1.1 0.30 2084 10 0.2 0.01 8.6 dioxane 3. 2 95.9 0.8 0. 10 18272
With ytterbium(III) triflate; In ethanol-d6; water-d2;Conversion of starting material; Example 2: Effect of Water to Ethanol ratio on Yb (OTf) 3 catalysed system Deuterated water (d2-water), deuterated ethanol (d6-ethanol) and ytterbium trifluoromethanesulfonate were mixed together according to the mass ratios in Table 2. A known quantity [OF Y-GLYCIDOXYPROPYLTRIMETHOXYSILANE] was added to the solution and the reaction was followed using proton nuclear magnetic resonance (NMR) spectroscopy. The time taken to 83% conversion was between 4 minutes and 174 minutes. There is a clear trend that for a given catalyst, with a fixed concentration of silane, for example [0.] 10 mol ratio, as the water percentage increases the reaction time increases. However, at near 100% water content, the reaction times decrease. Further experiments were carried out using 0.20 mol ratio, effectively doubling the silane concentration, and the same effects were observed. The apparent decrease in reaction time at near 100% water content implies that a different hydrolysis mechanism could be occurring. Table 2 Mol ratio Mol ratio Mol ratio Concentration Mass % Mass % Mass % Mass % Minutes to Water Silane Catalyst silane dm-3 Water Ethanol Silane catalyst 83% Conversion 5. 00 0. 10 0. 01 12. 91 6. 05 92.14 1.43 0. 37 4 10.00 0.10 0.01 12.91 11.96 86.26 1.41 0.37 47 25.00 0.10 0.01 12.91 28.88 69.40 1.36 0.36 159 50.00 0.10 0.01 12.91 54.64 43.73 1.29 0.34 174 99.89 0.10 0.01 12.91 98.53 0.00 1.16 0.31 81 10.00 0.20 0.01 8.60 4.06 94.86 0.96 0.13 29 50.00 0.20 0.01 25.54 53.99 43.13 2.55'0. 33 167 99.79 0. 20 0. 01 25.55 97. 54 0. 00 2. 31 0. 15 131
With ytterbium(III) triflate; In ethanol-d6; water-d2;Conversion of starting material; Example 5: Effect of Lanthanide Series Catalyst on Hydrolysis. Deuterated water (d2-water), deuterated ethanol and a series of lanthanide catalysts were mixed together according to the mass ratios in Table 5. A known quantity of [Y-GLYCIDOXYPROPYLTRIMETHOXYSILANE] was added to the solution and the reaction was followed using proton NMR spectroscopy. The time to 83% conversion was between 25 minutes and 272 minutes. All the lanthanide (III) (trifluoromethanesulfonate) 3 catalysts were active in hydrolysing [Y-GLYCIDOXYPROPYLTRIMETHOXYSILANE.] Table 5 Catalyst Mol ratio Mol ratio Mol ratio Concentration Mass %. Mass % Mass % Mass % Minutes to Water Silane catalyst silane Water Solvent Silane Catalyst 83% / g dm-3 Conversion LaTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 272 PrTFMS 10 0.2 0.01 8.60 4.1 89. 8 0.96 0.12 58 NdTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 63 SmTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 59 EuTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 43 GaTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 89 DyTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 61 ErTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 57 TmTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.12 63 YbTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.13 29 YbTFMS 10 0.2 0.01 8.60 4.1 89.8 0.96 0.13 25 [LA=LANTHANUM,] [PR=PRAESEODYMIUM,] Nd=neodymium, [SM=SAMARIUM,] [EU=EUROPIUM, GA=GADOIMIUM,] Dy=dysprosium, [ER=ERBIUM,] [TM=THULIUM,] Yb=ytterbium [TFMS=TRIFLUROMETHYLSULFONATE]
With ytterbium(III) triflate; In ethanol-d6; water-d2;Conversion of starting material; Example 6: Effect of Lanthanide Series Catalyst on Oligomerisation Deuterated water (d2-water), deuterated ethanol (d6-ethanol) and catalyst were mixed together according to the mass ratios in Table 6. A known quantity of y- glycidoxypropyltrimethoxysilane was added to the solution and the oligomerisation reaction was followed using silicon-29 NMR spectroscopy (measured by the rate of loss of monomeric species). Europium (III) and samarium [(III)] [TRIFLUOROMETHANESULFONATE,, WERE] the least effective oligomerisation catalysts and are the preferred catalysts where it is desired to avoid or to minimise oligomerisation, as, for example, in metal surface treatment processes. Ytterbium and erbium [(III)] tend to promote oligomerisation and hence these catalysts are more suitable for use in crosslinked gel formation processes, such as the generation of solgels, aerogels, xerogels and alcogels. Silicon-29 NMR measurements were performed at higher concentrations of silane and lower concentrations of water. The rate of oligomerisation at 1% mass of the silane (measured by proton NMR) is lower than the rate for 10% mass of silane when catalysed by Eu (III) trifluoromethanesulfonate (Table 6). This may also be the case for oligomerisation reactions catalysed by other metals in the lanthanide series. Table 6 Catalyst Mol ratio Mol ratio Mol ratio Concentration Mass % Mass % Mass % Mass % Half life of Water Silane catalyst Silane Water Solvent Silane Catalyst Silanetriol I g dm-3/mins EuTFMS 5 0. 2 0. 01 94. 20 21. 2 48. 9 10. 00 1. 27 141 EuTFMS 10 0.2 0.01 8.60 4.1 89.9 1.07 0.14 2143 YbTFMS 5 0.2 0.01 94.24 21.2 48.8 10.00 1.31 84 ErTFMS 5 0.2 0.01 94.20 21.2 48.9 10.00 1.30 131 SmTFMS 5 0.2 0.01 94.20 21.2 48.9 10.00 1.26 102 LaTFMS 5 0.2 0. 01 94.20 21. 2 48. 9 10. 00 1. 24 <80
With ytterbium(III) triflate; In [(2)H6]acetone; water-d2;Conversion of starting material; Example 3: Effect of solvent on Yb (OTf) 3 catalysed system Deuterated water (d2-water), deuterated solvent and ytterbium trifluoromethanesulfonate were mixed together according to the mass ratios in Table 3. A known quantity [OF Y-GLYCIDOXYPROPYLTRIMETHOXYSILANE] was added to the solution and the reaction was followed using proton NMR spectroscopy. The time taken to 83% conversion was between 23 minutes and 182752 minutes. Although the reaction was shown to take place in THF and dioxane, for industrial purposes, high concentrations of THF and dioxane are impracticable. It should be noted that the reaction proceeds faster in a more polar solvent and the best results are in protic solvents such as ethanol and methanol. Table 3 Mol ratio Mol ratio Mol ratio Concentration Solvent Mass Mass Mass Mass % Minutes to water silane catalyst silane % % % 83% /g dm-3 Water Solvent Silane Catalyst Conversion 10 0. 1 0. 01 12. 9 EtOD 12. 0 86.3 1.4 0. 37 47 10 0.2 0.01 8.6 EtOD 4.1 94.9 1.0 0.13 29 10 0.1 0.01 12.9 MeOD 12.0 86.3 1.4 0.37 58 10 0.2 0.01 8.6 MeOD 4.1 94.9 1.0 0.13 23 10 0.1 0.01 12.9 THF 10.9 87.4 1.3 0.34 416 10 0.2 0.01 8.6 THF 3.7 95.3 0.9 0.11 2682 10 0.1 0.01 12.9 D6-Acetone 12.2 86.0 1.4 0.38 173 10 0.2 0.01 8.6 D6-Acetone 4.1 94.8 1.0 0.13 267 10 0.1 0.01 12.9 ACN 12.5 85.6 1.5 0.39 142 10 0.2 0.01 8.6 ACN 4.3 94.6 1.0 0.13 124 10 0.1 0.01 12.9 dioxane 9.7 88.9 1.1 0.30 2084 10 0.2 0.01 8.6 dioxane 3. 2 95.9 0.8 0. 10 18272
With ytterbium(III) triflate; In ethyl [2]alcohol; water-d2;Conversion of starting material; Example 3: Effect of solvent on Yb (OTf) 3 catalysed system Deuterated water (d2-water), deuterated solvent and ytterbium trifluoromethanesulfonate were mixed together according to the mass ratios in Table 3. A known quantity [OF Y-GLYCIDOXYPROPYLTRIMETHOXYSILANE] was added to the solution and the reaction was followed using proton NMR spectroscopy. The time taken to 83% conversion was between 23 minutes and 182752 minutes. Although the reaction was shown to take place in THF and dioxane, for industrial purposes, high concentrations of THF and dioxane are impracticable. It should be noted that the reaction proceeds faster in a more polar solvent and the best results are in protic solvents such as ethanol and methanol. Table 3 Mol ratio Mol ratio Mol ratio Concentration Solvent Mass Mass Mass Mass % Minutes to water silane catalyst silane % % % 83% /g dm-3 Water Solvent Silane Catalyst Conversion 10 0. 1 0. 01 12. 9 EtOD 12. 0 86.3 1.4 0. 37 47 10 0.2 0.01 8.6 EtOD 4.1 94.9 1.0 0.13 29 10 0.1 0.01 12.9 MeOD 12.0 86.3 1.4 0.37 58 10 0.2 0.01 8.6 MeOD 4.1 94.9 1.0 0.13 23 10 0.1 0.01 12.9 THF 10.9 87.4 1.3 0.34 416 10 0.2 0.01 8.6 THF 3.7 95.3 0.9 0.11 2682 10 0.1 0.01 12.9 D6-Acetone 12.2 86.0 1.4 0.38 173 10 0.2 0.01 8.6 D6-Acetone 4.1 94.8 1.0 0.13 267 10 0.1 0.01 12.9 ACN 12.5 85.6 1.5 0.39 142 10 0.2 0.01 8.6 ACN 4.3 94.6 1.0 0.13 124 10 0.1 0.01 12.9 dioxane 9.7 88.9 1.1 0.30 2084 10 0.2 0.01 8.6 dioxane 3. 2 95.9 0.8 0. 10 18272
With ytterbium(III) triflate; In water-d2;Conversion of starting material; Example 2: Effect of Water to Ethanol ratio on Yb (OTf) 3 catalysed system Deuterated water (d2-water), deuterated ethanol (d6-ethanol) and ytterbium trifluoromethanesulfonate were mixed together according to the mass ratios in Table 2. A known quantity [OF Y-GLYCIDOXYPROPYLTRIMETHOXYSILANE] was added to the solution and the reaction was followed using proton nuclear magnetic resonance (NMR) spectroscopy. The time taken to 83% conversion was between 4 minutes and 174 minutes. There is a clear trend that for a given catalyst, with a fixed concentration of silane, for example [0.] 10 mol ratio, as the water percentage increases the reaction time increases. However, at near 100% water content, the reaction times decrease. Further experiments were carried out using 0.20 mol ratio, effectively doubling the silane concentration, and the same effects were observed. The apparent decrease in reaction time at near 100% water content implies that a different hydrolysis mechanism could be occurring. Table 2 Mol ratio Mol ratio Mol ratio Concentration Mass % Mass % Mass % Mass % Minutes to Water Silane Catalyst silane dm-3 Water Ethanol Silane catalyst 83% Conversion 5. 00 0. 10 0. 01 12. 91 6. 05 92.14 1.43 0. 37 4 10.00 0.10 0.01 12.91 11.96 86.26 1.41 0.37 47 25.00 0.10 0.01 12.91 28.88 69.40 1.36 0.36 159 50.00 0.10 0.01 12.91 54.64 43.73 1.29 0.34 174 99.89 0.10 0.01 12.91 98.53 0.00 1.16 0.31 81 10.00 0.20 0.01 8.60 4.06 94.86 0.96 0.13 29 50.00 0.20 0.01 25.54 53.99 43.13 2.55'0. 33 167 99.79 0. 20 0. 01 25.55 97. 54 0. 00 2. 31 0. 15 131
In ethanol; water;Reactivity (does not react); Example 1: (Comparative) Hydrolysis of GPS in water is catalysed by addition of acid or base, otherwise the rate of reaction is too slow to warrant use in an industrial process (see Table 1). Addition of ethanol or other solvent rapidly decreases the rate of hydrolysis to unacceptable levels. The addition of acetic acid to high ethanol to water ratio solutions, does not increase the rate of silane hydrolysis. Table 1 Mass % Mass % Mass % PH Minutes to Water Ethanol Silane 83% Conversion 99 0 1 Neutral 2200 99 0 1 4.3 68 99 0 1 9.0 381 4 95 1 Neutral >60000 59 40 1 Neutral 49000
A 20 ml scintillation bottle was initially charged with 9.4 g of Dynasylan GLYMO, 0.188 g of boric acid were added with stirring (magnetic stirrer), the mixture was heated at 60 C. for 30 minutes and then 0.864 g of demineralized water was stirred in. The mixture was stirred at a bottom temperature of 60 to 70 C. for a further 24 hours.A colorless, clear, low-viscosity liquid was obtained with a content (GC-TCD) of silane monomer of 14 area % (FIG. 4).

  • 14
  • [ 2530-83-8 ]
  • glycidoxypropyl silica [ No CAS ]
  • 15
  • [ 2530-83-8 ]
  • polysilsesquioxane; monomer: (3-glycidylpropyl) trimethoxysilane [ No CAS ]
  • 16
  • [ 2530-83-8 ]
  • carboxy-terminated poly(tert-butyl acrylate), Mn = 42000 Da, Mw = 47000 Da [ No CAS ]
  • poly(tert-butyl acrylate) grafted on 3-glycidoxypropyltrimethoxysilane [ No CAS ]
  • 17
  • [ 78-10-4 ]
  • [ 2530-83-8 ]
  • polymer; monomer(s): (3-glycidyloxypropyl)trimethoxysilane; tetraethoxysilane [ No CAS ]
  • 18
  • [ 2016-57-1 ]
  • [ 2530-83-8 ]
  • polymer, product of hydrolytic sol-gel polycondensation in bulk with 5-fold decylamine excess at 25 deg C for 3 min; monomer(s): [3-(glycidyloxy)propyl]trimethoxysilane; decylamine [ No CAS ]
  • 19
  • [ 2016-57-1 ]
  • [ 2530-83-8 ]
  • polymer, product of hydrolytic sol-gel polycondensation in bulk with 5-fold decylamine excess at 25 deg C for 1 h; monomer(s): [3-(glycidyloxy)propyl]trimethoxysilane; decylamine [ No CAS ]
  • 20
  • [ 2016-57-1 ]
  • [ 2530-83-8 ]
  • polymer, product of hydrolytic sol-gel polycondensation in bulk with 5-fold decylamine excess at 25 deg C for 4.5 h; monomer(s): [3-(glycidyloxy)propyl]trimethoxysilane; decylamine [ No CAS ]
  • 21
  • [ 2016-57-1 ]
  • [ 2530-83-8 ]
  • polymer, product of hydrolytic sol-gel polycondensation in bulk with 5-fold decylamine excess at 25 deg C for 24 h; monomer(s): [3-(glycidyloxy)propyl]trimethoxysilane; decylamine [ No CAS ]
  • 22
  • [ 2530-83-8 ]
  • polymer, product of hydrolytic polycondensation in bulk in presence of 1 percent p-toluenesulfonic acid at 20 deg C; monomer(s): [3-(glycidyloxy)propyl]trimethoxysilane [ No CAS ]
  • 23
  • [ 2530-83-8 ]
  • polymer, product of hydrolytic polycondensation in presence of benzyldimethylamine at 20 deg C for 10 min; monomer(s): [3-(glycidyloxy)propyl]trimethoxysilane [ No CAS ]
  • 24
  • [ 2530-83-8 ]
  • polymer, product of hydrolytic polycondensation in bulk in presence of 1 percent p-toluenesulfonic acid and benzyldimethylamine at 20 deg C for 24 h; monomer(s): [3-(glycidyloxy)propyl]trimethoxysilane [ No CAS ]
  • 25
  • [ 5807-14-7 ]
  • [ 2530-83-8 ]
  • C16H33N3O5Si [ No CAS ]
  • 26
  • [ 124-38-9 ]
  • [ 2530-83-8 ]
  • 4-((3-(trimethoxysilyl)propoxy)methyl)-1,3-dioxolan-2-one [ No CAS ]
  • 27
  • [ 2530-83-8 ]
  • 1-[Bis-(2-hydroxy-ethyl)-amino]-3-[3-(2,8,9-trioxa-5-aza-1-sila-bicyclo[3.3.3]undec-1-yl)-propoxy]-propan-2-ol [ No CAS ]
  • 28
  • [ 2530-83-8 ]
  • 1-(3-Oxiranylmethoxy-propyl)-3-[3-(2,8,9-trioxa-5-aza-1-sila-bicyclo[3.3.3]undec-1-yl)-propoxymethyl]-2,8,9-trioxa-5-aza-1-sila-bicyclo[3.3.3]undecane [ No CAS ]
  • 29
  • [ 2530-83-8 ]
  • 1-{2-Hydroxy-3-[3-(3,7,10-trimethyl-2,8,9-trioxa-5-aza-1-sila-bicyclo[3.3.3]undec-1-yl)-propoxy]-propylamino}-3-[3-(3,7,10-trimethyl-2,8,9-trioxa-5-aza-1-sila-bicyclo[3.3.3]undec-1-yl)-propoxy]-propan-2-ol [ No CAS ]
  • 30
  • [ 2530-83-8 ]
  • 1-(Bis-{2-hydroxy-3-[3-(3,7,10-trimethyl-2,8,9-trioxa-5-aza-1-sila-bicyclo[3.3.3]undec-1-yl)-propoxy]-propyl}-amino)-3-[3-(3,7,10-trimethyl-2,8,9-trioxa-5-aza-1-sila-bicyclo[3.3.3]undec-1-yl)-propoxy]-propan-2-ol [ No CAS ]
  • 32
  • [ 288-32-4 ]
  • [ 2530-83-8 ]
  • [ 149394-77-4 ]
  • [ 149394-70-7 ]
  • [ 149394-84-3 ]
YieldReaction ConditionsOperation in experiment
at 95℃; for 1.5h; 13.62 g (0.2 mol) of imidazole was melted at 95C, and 47.27 g (0.2 mol) of (3-glycidoxypropyl)trimethoxysilane was added dropwise thereto over a period of 30 minutes while stirred in an argon atmosphere. Following addition, the product was further reacted for one hour at a temperature of 95C, yielding an imidazole group-containing silane coupling agent comprising a mixture of the compounds represented by the chemical formulas (1), (2) and, (3) below. In the formulas (1), (2), and (3) below, R1, R2, and R3 are H; R4 is CH3; n is 3; and m is 3. 12.16 g (0.04 mol) of the imidazole group-containing silane coupling agent thus obtained, 8.64 g (0.06 mol) of 2-phenylimidazole (melting point: 137-147C), and 21.0 g (0.1 mol) of trimellitic acid were heated and mixed at 160C, the reaction was continued for one hour, and the product was cooled to room temperature, yielding an imidazole trimellitate composition that was solid at normal temperature. The solid product thus obtained was ground with a mortar and classified by a sieve with hole openings of 90 microns to yield pulverized Sample No. 1.
at 95℃; for 1.5h; 13.62 g (0.2 mol) of imidazole was melted at 95C, and 47.27 g (0.2 mol) of (3-glycidoxypropyl)trimethoxysilane was added dropwise thereto over a period of 30 minutes while stirred in an argon atmosphere. Following addition, the product was further reacted for one hour at a temperature of 95C, yielding an imidazole group-containing silane coupling agent comprising a mixture of the compounds represented by the chemical formulas (5), (6), and (7) below. 30.4 g (0.1 mol) of the imidazole group-containing silane coupling agent thus obtained and 25.4 g (0.1 mol) of pyromellitic acid were heated and mixed at 120C, and an imidazole group-containing silane coupling agent pyromellitate was obtained by continuing the reaction for one hour. 20.8 g of phenol resin (Phenolite TD-2093 having a softening point of 100C, mfd. by Dainippon Ink and Chemicals, Inc.) was added to this carboxylate, the product was heated and mixed for one hour at 120C, and an imidazole group-containing silane coupling agent pyromellitate/phenol resin composition that was solid at normal temperature was obtained by cooling the product to room temperature. The solid product thus obtained was ground with a mortar and classified by a sieve with hole openings of 90 microns to yield pulverized Sample No. 1.
  • 33
  • [ 3236-54-2 ]
  • [ 2530-83-8 ]
  • TG13 [ No CAS ]
YieldReaction ConditionsOperation in experiment
A 3:1 molar ratio of <strong>[2530-83-8]3-glycidoxypropyltrimethoxysilane</strong>(GPS) and C,C,C-trimethyl-1,6-hexanediamine(TMH) is added to an equal weight of ethyl alcohol. The mixture is allowed to react at 70 C. for 3 hours. The reaction products are subsequently neutralized with a 20% excess (based on stoichiometry) of acetic acid.
  • 34
  • [ 3236-54-2 ]
  • [ 2530-83-8 ]
  • TG14 [ No CAS ]
YieldReaction ConditionsOperation in experiment
A 4:1 molar ratio of <strong>[2530-83-8]3-glycidoxypropyltrimethoxysilane</strong>(GPS) and C,C,C-trimethyl-1,6-hexanediamine(TMH) is added to an equal weight of ethyl alcohol. The mixture is allowed to react at 70 C. for 3 hours. The reaction products are subsequently neutralized with a 20% excess (based on stoichiometry) of acetic acid.
  • 35
  • [ 112926-00-8 ]
  • [ 2530-83-8 ]
  • C6H13O5PolSi [ No CAS ]
YieldReaction ConditionsOperation in experiment
In toluene; for 50h;Heating / reflux; [117] Synthesis Example 1: Synthesis of silica gel of formula 2 where R is 3-glycidoxypropyl group [118] Ig of a silica gel was dried at 100 C under reduced pressure for 12 hours and 20 mL of toluene was added thereto. 5 mL of <strong>[2530-83-8]3-glycidoxypropyltrimethoxysilane</strong> was added to the mixed solution, refluxed for 50 hours, washed with toluene, methanol, acetone, and diethylether, and dried under reduced pressure, to give a modified silica gel of formula 2 where R is a 3-glycidoxypropyl group. [119] ¹³ C CP MAS NMR (75MHz): 6 = 75.0,66.5, 61.9, 56.5, 10.1.
  • 36
  • C48H46N26O12 [ No CAS ]
  • [ 2530-83-8 ]
  • C66H86N26O22Si2 [ No CAS ]
YieldReaction ConditionsOperation in experiment
In dimethyl sulfoxide; at 80℃; for 30h; [123] Synthesis Example 3: Synthesis of silane compound of formula 8 where n=5 and m=3 [124] 2.9 g of diaminophenylcucurbit [6] uril of formula 1 where n=5 and R=3-aminopheyl group was dissolved in 40 mL of dimethylsulfoxide. Then, 1.1 mL of <strong>[2530-83-8]3-glycidoxypropyltrimethoxysilane</strong> was added thereto and stirred at 80 C for 30 hours. [125] After the reaction terminated, a precipitate was removed by addition of acetone. Then, the resultant solution was washed with acetone and diethylether and dried to give a disubstituted cucurbituril-bonded silane compound of formula 8 where n=5 and m=3. [126] ¹ H NMR (500MHz, DMSO-d 6) : No. = 0.71(t , J = 15Hz), 1.84 (m), 3.45(s), 3.60 (m), 3.97 (m), 4.02 (m), 4.43 (m), 5.27 (d, J = 10.0), 5.56 (d, J = 10.0 Hz), 5.70 (m), 5.80 (m), 5.97 (t, J = 15.0 Hz), 6.26 (s), 6.39 (m), 6.62 (m), 7.04 (m).
  • 37
  • [ 106-92-3 ]
  • [ 2487-90-3 ]
  • [ 2530-83-8 ]
YieldReaction ConditionsOperation in experiment
82% Preparation of Preparation of silane compound by hydrosilylation of trimethoxysilane and allyl glycidyl ether A catalyst described in Table 1 (20 ppm (1.2×10-6 mol) of platinum included in the catalyst) was dissolved in xylene and added to a 25 mL 2-necked round-bottom flask equipped with a nitrogen gas inlet tube and a cooling tube. After adding trimethoxysilane (6.43 g, 52.6 mmol) and dodecane (0.5 g, 2.9 mmol) as internal standard, the mixture was stirred for 5 minutes under reflux. Then, allyl glycidyl ether (5.00 g, 43.8 mmol) was added dropwisely at a rate of 1 mL/min using a syringe. Thereafter, the progress of reaction was monitored by gas chromatography.The hydrosilylation reaction of Preparation Example 5 was performed according to Scheme 8. Reaction condition and yield of the produced silane compound are given in Table 6.[Scheme 8] Used catalyst amount Reaction condition Remaining allyl glycidyl ether (%) Product Temp. (ºC) Time (hr) Yield (%) Comp. Ex. 1 20 ppm reflux 2 92 5 Ex. 1 20 ppm reflux 2 16 82
80% EXAMPLE 8 A three-neck flask equipped with a reflux condenser, stirring rod and thermometer was charged with 11.4 grams of allyl glycidyl ether (0.1 mole) and one cubic centimeter of Catalyst A of Example 1 as a catalyst (10min5 mole on a platinum basis). 13.4 grams of trimethoxy silane (0.11) were dropwise added in one hour from a dropping funnel. The reaction temperature was maintained at 50C. The reaction was further carried out for 30 minutes. The gas chromatography analysis demonstrated that gamma-glycidyloxypropyl trimethoxy silane was obtained in a yield of 80% on an allyl glycidylether basis.
dihydrogen hexachloroplatinate(IV) hexahydrate; In acetone; at 20 - 130℃; under 18751.9 Torr;Inert atmosphere; EXAMPLEPreparation of 3-glycidyloxypropyltrimethoxysilaneThe system used for the preparation of 3-glycidyloxypropyltrimethoxysilane consisted essentially of the reactant reservoir vessels, diaphragm pumps, control, measurement, and metering units, a T mixer, two replaceable preliminary reactors, connected in parallel and packed with packing elements (stainless steel beads with an average diameter of 1.5 mm) (diameter 5 mm, length 40 mm, stainless steel), a stainless-steel capillary (1 mm in diameter, 50 m in length), a thermostat bath with temperature regulation for the preliminary reactors and capillary, a pressure maintenance valve, a stripping column operated continuously with N2, and the lines needed for supplying reactant and also for removing product, recyclate, and offgas. First of all, at room temperature, the olefin (allyl glycidyl ether) and platinum catalyst [53 g of hexachloroplatinic acid hexahydrate in 1 l of acetone] were metered in a molar olefin:Pt ratio of 270 000:1 and mixed and this mixture was mixed in the T mixer with hydrogen trimethoxysilane (TMOS), Degussa AG in a molar TMOS:olefin ratio of 0.9:1, and supplied continuously to the reactor system. The pressure was 25+/-10 bar. When the system is being run up, the aim ought to be for a very highly H2O- and O2-free condition of the system. Further, before the temperature in the reactor system was raised, the system was flushed with reactant mixture A+C for 2 hours. At a continuous throughput totaling 300 g/h, the temperature in the thermal conditioning bath was raised, set at 130 C. in the reactor system and operated continuously over 14 days. After the reactor system, samples were taken from the crude product stream at intervals of time and were analyzed by means of GC-WLD measurements. The conversion, based on TMOS, was 79%, and the selectivity, based on the target product, was around 86%. The stream of reaction product thus obtained was supplied continuously to a stripping column operated with N2, and hydrosilylation product was taken off continuously.
C13H28N2OPtSi2; In dodecane; xylene; for 0.0333333h;Inert atmosphere; Reflux;Product distribution / selectivity; A catalyst described in Table 1 (20 ppm (1.2×10-6 mol) of platinum included in the catalyst) was dissolved in xylene and added to a 25 mL 2-necked round-bottom flask equipped with a nitrogen gas inlet tube and a cooling tube. After adding trimethoxysilane (6.43 g, 52.6 mmol) and dodecane (0.5 g, 2.9 mmol) as internal standard, the mixture was stirred for 5 minutes under reflux. Then, allyl glycidyl ether (5.00 g, 43.8 mmol) was added dropwisely at a rate of 1 mL/min using a syringe. Thereafter, the progress of reaction was monitored by gas chromatography.The hydrosilylation reaction of Preparation Example 5 was performed according to Scheme 8. Reaction condition and yield of the produced silane compound are given in Table 6.
With dihydrogen hexachloroplatinate(IV) hexahydrate; In tetrahydrofuran; isopropyl alcohol; at 90℃; The raw material is trimet oxygen radical hydrogen silicon and allyl glycidyl ether, the main catalyst is of the six-hydrated chloroplatinic acid, compounding chemicals as tetrahydrofuran and isopropanol, three a oxygen radical hydrogen silicon, allyl glycidyl ether and six hydrated chloroplatinic acid in a molar ratio of 400000:400000: 1, six hydration volume ratio of chloroplatinic acid with 9:1 to prepare mixed solution of tetrahydrofuran and isopropanol 1 the solution [...] ; channel reaction device is a baffle, an activator is organic amine, channel inner diameter is 6 mm, the length is 60 m, the velocity of flow of the reaction stream is 25 kg/h, the reaction temperature 90 C; the catalyst mixture is fully mixed with the allyl glycidyl ether, the three a oxygen radical hydrogen silicon at the same time with the allyl glycidyl ether reaction from the channel and pumped into two entrance of the device. From the passage the outlet of the reaction device for sampling and testing, the results of 3 - (2,3-epoxypropoxy) propyl trimethoxy silane content is 82.6%, three a oxygen radical hydrogen silicon 1.9%, allyl glycidyl ether 1.02%.

  • 38
  • aluminum(III) nitrate nonahydrate [ No CAS ]
  • titanium(IV) tetraethanolate [ No CAS ]
  • neodymium(III) nitrate hexahydrate [ No CAS ]
  • [ 2530-83-8 ]
  • O2Si(50),O2Ti(50),AlO1.5(10),NdO1.5(1) (A) [ No CAS ]
  • 39
  • [ 2530-83-8 ]
  • C7H16O5Si [ No CAS ]
YieldReaction ConditionsOperation in experiment
With water; at 20℃; for 1h;pH 7; A 40% solution of silane (F-3) at pH=7 is used.12.5 g of this 40% solution are poured into a beaker and made up with 200 g of demineralized water. 200 g of untreated filler (B-1) are poured into this solution and the mixture is stirred for 1 hour at room temperature using an impeller stirrer. The mixture is poured into a crystallizing dish and the filler is dried in an oven for 16 hours at 150 C. The filler is then screened through a 250 micron gauze.
  • 40
  • [ 2530-83-8 ]
  • [ 869857-36-3 ]
YieldReaction ConditionsOperation in experiment
With water; at 20℃; for 1h;pH 3 - 4;Acidic conditions; The solution used is a solution containing 40% silane (F-2) with a pH=3-4.12.5 g of this 40% solution of silane (F-2) are poured into a beaker and made up with 200 g of demineralized water. 200 g of filler (B-1) are poured into this solution and the mixture is stirred for 1 hour at room temperature using an impeller stirrer. The mixture is poured into a crystallizing dish and the filler is dried in an oven for 16 hours at 150 C. The filler is then screened through a 250 micron gauze.
  • 41
  • [ 30418-59-8 ]
  • [ 2530-83-8 ]
  • [ 100340-93-0 ]
  • 42
  • [ 2530-83-8 ]
  • C6H11O2Pol [ No CAS ]
YieldReaction ConditionsOperation in experiment
With 2?chlorotrityl chloride resin; triethylamine; In toluene; at 20℃; for 20h;Product distribution / selectivity; 39 g of toluene (Junsei Chemical), 450 mul of <strong>[2530-83-8]3-glycidoxypropyltrimethoxysilane</strong> (TSL8350, GE Toshiba Silicone), 900 mul of triethylamine (Wako Pure Chemical Industries) were mixed, and a 10 cm square UV-cleansed glass substrate (NA35, NH Technoglass) was immersed in it and shaken mildly for 20 hours at room temperature. After that, the substrate was washed with ethanol and water and nitrogen blow-dried. Epoxy groups were introduced on the glass surface by this operation. Next, the glass substrate was immersed in TEG (Kanto Chemical) containing a catalytic amount of concentrated sulfuric acid and heated for 1 hour at 80 C. After this reaction, the substrate was washed well with water and nitrogen blow-dried. By this operation, the TEG reacted with the epoxy groups and formed covalent bonds. Next, 100 mg of anhydrous succinic acid (SuA, Kanto Chemical) and 120 mg of 4-dimethylaminopyridine (DMAP, Wako Pure Chemical Industries) were dissolved in 43 g of toluene, the above substrate immersed in it, and heated for 1 hour at 80 C. After that, the substrate was washed with ethanol and water, and nitrogen blow-dried. The ring-opening half-esterification reaction advanced in this step and carboxyl groups were introduced on the free ends of the TEG. Next, 290 mg of N-hydroxysuccinimide (NHS, Wako Pure Chemical Industries) and 390 mul of N,N'-diisopropylcarbodiimide (DIC, Wako Pure Chemical Industries) were dissolved in 47 g of N,N'-dimethylformamide (DMF, Kanto Chemical), and the substrate was immersed in it and heated for 1 hour at 80 C. After that, the substrate was washed with ethanol and water, and nitrogen blow-dried. N-hydroxysuccinimide (NHS) groups were introduced at the free ends of the TEG by this operation. Lastly, the substrate was cut into pieces of size 25 mm×10 mm.; Example 2 The Example shown in FIG. 5 comprises a step of introducing aldehyde groups on a glass surface, a step of covalent bonding of TEG to the aldehyde group, a step of reacting anhydrous succinic acid with the hydroxyl groups present at the free ends of the TEG to form carboxyl groups, a step of converting the carboxyl groups into active esters, a step of making a protein to act on active esters, and a step of inactivating the unreacted active esters using ethanolamine. The specific procedures used are described below.39 g of toluene, 450 mul of <strong>[2530-83-8]3-glycidoxypropyltrimethoxysilane</strong>, and 900 mul of triethylamine were mixed, and a 10 cm square UV-cleansed glass substrate was immersed in it and shaken mildly for 20 hours at room temperature. After that, the substrate was washed with ethanol and water and nitrogen blow-dried. Epoxy groups were introduced on the glass surface by this procedure. In the next step, the substrate was immersed in dilute (10 mM) sulfuric acid and heated for 2 hour at 80 C. After this, the substrate was washed well with water and nitrogen blow-dried. By this operation, the epoxy groups were hydrolyzed and 1,2-diols were formed. Next, the substrate was immersed in 20 mM aqueous sodium periodate solution (Kanto Chemical), left standing for 15 minutes at room temperature, and washed with water. By this operation, the 1,2-diols underwent oxidative cleavage to form aldehyde groups. After that, the substrate was immersed in TEG containing catalytic amounts of concentrated sulfuric acid and heated for 1 hour at 80 C. The substrate was then washed well with water and nitrogen blow-dried. In this step, the TEG reacted with the aldehyde groups to form covalent bonds. Next, 100 mg of SuA and 120 mg DMAP were dissolved in 43 g of toluene, and the above substrate was immersed in it and heated for 1 hour at 80 C. The substrate was then washed with ethanol and water and nitrogen blow-dried. This step formed carboxyl groups on the free ends of the TEG. Next, 290 mg of NHS and 390 mul of DIC were dissolved in 47 g of DMF, and the substrate was immersed in it and heated for 1 hour at 80 C. After that, the substrate was washed with ethanol and water and nitrogen blow-dried. NHS groups were introduced at the free ends of the TEG by this operation. Lastly, the substrate was cut into pieces of size 25 mm×10 mm.; Example 3 To apply the present invention effectively, it is very important to use a suitable catalyst in the carboxyl group-forming step. The results of experiments on which the above statement is based are described below. 39 g of toluene, 450 mul of <strong>[2530-83-8]3-glycidoxypropyltrimethoxysilane</strong>, and 900 mul of triethylamine were mixed, and a 10 cm square UV-cleansed glass substrate was immersed in it and shaken mildly for 20 hours at room temperature. After that, the substrate was washed with ethanol and water and nitrogen blow-dried. Epoxy groups were introduced on the glass surface by this operation. Next, the above substrate was immersed in TEG containing a catalytic amount of concentrated sulfuric acid and heated for 1 hour at 80 C. After this reaction, the substrate was washed well with water and nitrogen blow-dried. In this operation,...
Firstly, 39 g of toluene (Junsei Chemical), 450 mul of <strong>[2530-83-8]3-glycidoxypropyltrimethoxysilane</strong> (TSL8350, GE Toshiba Silicone), and 900 mul of triethylamine (Wako Pure Chemical Industries) were mixed, and a 10 cm square UV-cleansed glass substrate (NA35, NH Technoglass) was immersed in it and shaken mildly for 20 hours at room temperature. After that, the substrate was washed with ethanol and water and nitrogen blow-dried. On the other hand, functional groups were introduced on a glass surface by the sol-gel method as follows. Firstly, 2205 mul of <strong>[2530-83-8]3-glycidoxypropyltrimethoxysilane</strong> (TSL8350, GE Toshiba Silicone) and 480 mul of 0.005 N hydrochloric acid were mixed and stirred for 1 hour. This was diluted with isopropyl alcohol to prepare a 0.25% sol solution. A glass substrate (NA35, NH Technoglass) was coated with this by spin coating. The number of revolutions was set at 1000 rpm, and the revolution time at 3 seconds. After drying for a while, the substrate was heated for 20 minutes in an oven at 80 C. Each of these glass substrates silane-treated by the different methods was immersed in TEG (Kanto Chemical) containing a catalytic amount of concentrated sulfuric acid and heated for 1 hour at 80 C. After this reaction, the substrate was washed well with water and nitrogen blow-dried. Next, 100 mg of anhydrous succinic acid (SuA, Kanto Chemical) and 120 mg of 4-dimethylaminopyridine (DMAP, Wako Pure Chemical Industries) were dissolved in 43 g of toluene, the above substrate immersed in it, and heated for 1 hour at 80 C. After that, the substrate was washed with ethanol and water, and nitrogen blow-dried. Next, 290 mg of N-hydroxysuccinimide (NHS, Wako Pure Chemical Industries) and 390 mul of N,N'-diisopropylcarbodiimide (DIC, Wako Pure Chemical Industries) were dissolved in 47 g of N,N'-dimethylformamide (DMF, Kanto Chemical), and the substrate was immersed in it and heated for 1 hour at 80 C. The substrate was washed with ethanol and water, and nitrogen blow-dried. After that, the substrate was cut into pieces of size 25 mm×10 mm. Two substance immobilizing carriers differing only in the method of applying the silane coupling agent were obtained by the above-described procedures.
  • 43
  • [ 2530-83-8 ]
  • [ 113231-05-3 ]
  • C19H38N2O11Si [ No CAS ]
  • 44
  • [ 38521-46-9 ]
  • [ 2530-83-8 ]
  • [ 1190597-62-6 ]
  • 45
  • [ 106-92-3 ]
  • [ 2487-90-3 ]
  • [ 2530-83-8 ]
  • (Z)-1-propenyl glycidyl ether [ No CAS ]
YieldReaction ConditionsOperation in experiment
With acetic acid;platinum(0)-1,3-divinyl-1,1,3,3-tetramethyldisiloxane complex; at 160℃;tube reactor;Product distribution / selectivity; In the example, allyl glycidyl ether was reacted with trimethoxysilane to form 3-glycidyloxypropyltrimethoxysilane. The reaction was carried out continuously by feeding the raw materials (allyl glycidyl ether: 9.6 kg/h and trimethoxysilane: 8 kg/h) together with the Pt Karstedt catalyst in the presence of acetic acid (0.05% by weight, based on the total mass of reactants) into a tube reactor. The concentration of the catalyst based on metallic platinum was 2 ppm. The Pt Karstedt catalyst was dissolved in 3-glycidyloxypropyltrimethoxysilane. The reaction temperature was about 160 C. The reaction was carried out using an excess of allyl glycidyl ether (molar ratio of allyl glycidyl ether:trimethoxysilane=1.28:1). The reaction mixture formed was composed of: cis-iso- trans-iso- iso- cyclo- TMOS DYN M AGE AGE AGE GLYMO GLYMO GLYMO HB [%] [%] [%] [%] [%] [%] [%] [%] [%] 0.2 0.4 0.4 6.4 3 0.3 0.1 87.3 1.9 TMOS = trimethoxysilane DYN M = tetramethoxysilane AGE = allyl glycidyl ether cis-iso-AGE = cis-propenyl glycidyl ether trans-iso-AGE = trans-propenyl glycidyl ether iso-GLYMO = 2-glycidyloxy-1-methylethyltrimethoxysilane cyclo-GLYMO = 1-dimethoxysila-2,5-dioxa-3-methoxymethylcyclooctane GLYMO = 3-glycidyloxypropyltrimethoxysilane HB = high boilersThe composition of the product mixture was determined by means of gas chromatography.
With platinum(0)-1,3-divinyl-1,1,3,3-tetramethyldisiloxane complex; 2-Ethylhexanoic acid; at 100℃; for 2h;Catalytic behavior; The experiments which follow (comparative experiments 2 to 7 and inventive experiments 1 to 8) were conducted as follows: AGE, TMOS, acid and Karstedt catalyst were initially charged in a stirred reactor. The reaction mixture was heated up to 100 C. (bottom temperature) while stirring within about 30 min. After the bottom temperature of 100 C. had been attained, the reaction mixture was kept at 100 C. for a further 90 min. Thereafter, the reaction mixture/product mixture was cooled down and then a sample was taken (called the crude sample). The crude product obtained was then fractionally distilled under product-conserving conditions (reduced pressure) and the target product was obtained as the top product.
  • 46
  • [ 106-92-3 ]
  • [ 2487-90-3 ]
  • [ 2530-83-8 ]
  • (Z)-1-propenyl glycidyl ether [ No CAS ]
  • (E)-1-propenyl glycidyl ether [ No CAS ]
YieldReaction ConditionsOperation in experiment
platinum(0)-1,3-divinyl-1,1,3,3-tetramethyldisiloxane complex; at 160℃;tube reactor;Product distribution / selectivity; In the example, allyl glycidyl ether was reacted with trimethoxysilane to form 3-glycidyloxypropyltrimethoxysilane. The reaction was carried out continuously by feeding the raw materials (allyl glycidyl ether: 9.6 kg/h and trimethoxysilane: 8 kg/h) together with the Pt Karstedt catalyst in the presence of acetic acid (0.05% by weight, based on the total mass of reactants) into a tube reactor. The concentration of the catalyst based on metallic platinum was 2 ppm. The Pt Karstedt catalyst was dissolved in 3-glycidyloxypropyltrimethoxysilane. The reaction temperature was about 160 C. The reaction was carried out using an excess of allyl glycidyl ether (molar ratio of allyl glycidyl ether:trimethoxysilane=1.28:1). The reaction mixture formed was composed of: cis-iso- trans-iso- iso- cyclo- TMOS DYN M AGE AGE AGE GLYMO GLYMO GLYMO HB [%] [%] [%] [%] [%] [%] [%] [%] [%] 0.2 0.4 0.4 6.4 3 0.3 0.1 87.3 1.9 TMOS = trimethoxysilane DYN M = tetramethoxysilane AGE = allyl glycidyl ether cis-iso-AGE = cis-propenyl glycidyl ether trans-iso-AGE = trans-propenyl glycidyl ether iso-GLYMO = 2-glycidyloxy-1-methylethyltrimethoxysilane cyclo-GLYMO = 1-dimethoxysila-2,5-dioxa-3-methoxymethylcyclooctane GLYMO = 3-glycidyloxypropyltrimethoxysilane HB = high boilersThe composition of the product mixture was determined by means of gas chromatography.When the above-described process is carried out without the use of acetic acid as promoter, the following reaction composition is obtained. cis-iso- trans-iso- iso- cyclo- TMOS DYN M AGE AGE AGE GLYMO GLYMO GLYMO HB [%] [%] [%] [%] [%] [%] [%] [%] [%] 0.3 1.15 1.7 6.35 6.35 1.1 0.15 81 1.9
With platinum(0)-1,3-divinyl-1,1,3,3-tetramethyldisiloxane complex; at 160℃; General procedure: Allyl glycidyl ether was reacted continuously with trimethoxysilane to give 14 3-glycidyloxypropyltrimethoxysilane. The reaction was effected continuously in a tubular reactor by feeding in the raw materials (allyl glycidyl ether 9.6 kg/h and trimethoxysilane: 8 kg/h) together with the Pt Karstedt catalyst in the presence of acetic acid (0.05% by weight, based on the overall reaction mixture). The concentration of the catalyst based on metallic platinum was 2 ppm. The Pt Karstedt catalyst was dissolved in 3-glycidyloxypropyltrimethoxysilane. The reaction temperature was about 160 C. The reaction was run with an excess of allyl glycidyl ether (molar ratio: allyl glycidyl ether:trimethoxysilane=1.28:1). The product mixture obtained after reaction was composed of. The composition of the product mixture obtained after reaction was determined by means of gas chromatography. The present product mixture was distilled to obtain the end product, and the acetic acid content after distillation was still around 200 ppm by weight. When the process described above was conducted without the use of acetic acid as promoter, the following reaction product/crude product composition was obtained:
  • 47
  • [ 5036-48-6 ]
  • [ 2530-83-8 ]
  • [ 1204776-56-6 ]
YieldReaction ConditionsOperation in experiment
98% In tetrahydrofuran; at 95℃; for 6h;Inert atmosphere; Example 1 : Synthesis of Compound 1; [68] A Compound 1 represented by Formula 1 was synthesized according to Reaction; Scheme 1 below.[69] <Reaction Scheme 1>[70]^ - « ' ? v ; 1 (J-a»»illi> p«ij»j CMait&XOtt 5 tttrfatovprQp)Jfrin<riho»Hiiota<trLambdarc &fli-alphar > > [71] 162.68 g of tetrahydrofurane, 6.259 g (0.05 mol) of glycidoxypropy- ltrimethoxysilane, and 11.817 g (0.05 mol) of l-(3-aminopropyl)-imidazole were charged into a reactor and were reacted for 6 hours by maintaining the temperature of the reactor at 95 0C under a nitrogen atmosphere with rotating a mechanical stirrer at 300 rpm. After the reaction was completed, a solvent was removed from a resultant for 2 hours by using a rotary evaporator. Then the resultant was dried for 24 hours in a vacuum oven and 7 g (yield 98 %) of Compound 1 represented by Formula 1 was obtained thereby.[72] i H NMR (300 MHz) : delta 0.62~0.68(m, IH), 1.89~1.96(m ,8H), 1.64~1.67(t, 2H), ),2.54~2.56(t, 7H), 2.58~2.61(m, 6H), 3.28~3.31(m, SiOCH3) 3.38~3.40(d, 3H), 3.42~3.44(d,4H), .3.50~3.58(m, 5H), 3.64(s, -NH-), 3.80(s, OH), 4.05-4.10(m, 9H), 6.95(s, 10H), 7.12~7.13(t, HH), 7.65(s, 12H)[73] IR (neat, cm 1) : 3650~3200(vOH), 3300~3200(vNH), 1120~1050(vs,(alkoxy))
  • 48
  • [ 110-91-8 ]
  • [ 2530-83-8 ]
  • [ 1222257-39-7 ]
  • [ 1222257-40-0 ]
  • [ 1222257-42-2 ]
  • C25H54N2O11Si2 [ No CAS ]
YieldReaction ConditionsOperation in experiment
53% With sodium methylate; In methanol; toluene; at 116 - 140℃; A flask equipped with a stirrer, a Dean-Stark trap, a reflux condenser, a dropping funnel, and a thermometer was charged with 52 g (0.60 mole) of morpholine, 300 mL of toluene, and 1.5 g of solution of sodium methoxide in methanol (28% by weight of sodium methoxide), and 94 g (0.40 mole) of gamma-glycidoxypropyltrimethoxysilane was added dropwise while refluxing the toluene. The dropwise addition was continued for 8 hours while gradually removing the fraction containing the alcohol from the Dean-Stark trap, and during the addition, internal temperature of the flask was maintained at 116 to 119 C. Removal of the fraction was continued until the internal temperature was 140 C., and the reaction was completed. The resulting reaction mixture was a mixed composition containing the compounds general formulae (19) to (22), and analysis by gas chromatography confirmed that weight ratio of the compounds of formulae (19) to (22), namely, the compound of the formula (19):the compound of the formula (20):the compound of the formula (21):the compound of the formula (22) in the mixed composition was 52:6:10:32. The reaction mixture was distilled to obtain 59 g of a fraction having a boiling point of 134 to 136 C. at 0.3 kPa. The thus obtained fraction was evaluated by mass spectrum, 1H-NMR spectrum (deuterated chloroform solvent), and IR spectrum. The results of the mass spectrum are as shown below. FIG. 15 is the chart for the 1H-NMR spectrum, and FIG. 16 is the chart for the IR spectrum.Mass spectrum:m/z 291, 260, 204, 163, 100These results confirmed that the resulting compound was 1,1-dimethoxy-3-morpholinomethyl-2,5-dioxa-1-silacyclooctane, and the yield in terms of silicon was 53%.
  • 49
  • [ 109-01-3 ]
  • [ 2530-83-8 ]
  • [ 1222257-17-1 ]
  • [ 1222257-19-3 ]
  • [ 1222257-23-9 ]
  • [ 1222257-21-7 ]
YieldReaction ConditionsOperation in experiment
A flask equipped with a stirrer, a reflux condenser, a dropping funnel, and a thermometer was charged with 30 g (0.30 mole) of methylpiperazine, and 71 g (0.30 mole) of gamma-glycidoxypropyltrimethoxysilane was added dropwise at 85 to 95 C. for 4 hours, and the mixture was stirred at the same temperature for 2 hours to obtain a transparent composition.The resulting composition was evaluated for 1H-NMR spectrum (deuterated chloroform solvent) and IR spectrum. FIG. 1 is the chart for the 1H-NMR spectrum, and FIG. 2 is the chart for the IR spectrum. Mass spectrum was also measured after silylating the resulting composition with bis(trimethylsilyl)trifluoroacetamide. The results of the mass spectrum are shown below.Mass spectrum 1:m/z 408, 393, 318, 229, 121, 113Mass spectrum 2:m/z 304, 273, 234, 139, 113Mass spectrum 3:m/z 712, 640, 393, 318, 229, 121Mass spectrum 4:m/z 608, 593, 318, 273, 121, 113These results confirmed that the resulting composition was a mixed composition containing the compounds of the following formulae (7) to (10): The resulting composition after the silylation was also analyzed by gas chromatography. Weight ratio of the compounds of formulae (7) to (10), namely, the compound of the formula (7):the compound of the formula (8):the compound of the formula (9):the compound of the formula (10) in the mixed composition was confirmed to be 20:46:7:27.
  • 50
  • [ 109-01-3 ]
  • [ 2530-83-8 ]
  • [ 1222257-17-1 ]
  • [ 1222257-19-3 ]
  • [ 1222257-23-9 ]
YieldReaction ConditionsOperation in experiment
75% at 140 - 149℃;Product distribution / selectivity; A flask equipped with a stirrer, a thermometer, a packed column equipped at its upper end with a dropping funnel, a Dean-Stark trap, and a reflux condenser, and a thermometer was charged with 150 g (1.50 mole) of methylpiperazine and 60 g (0.30 mole) of gamma-glycidoxypropyltrimethoxysilane was added dropwise while refluxing the methylpiperazine. The dropwise addition was continued for 10 hours while gradually removing the methylpiperazine containing the alcohol from the Dean-Stark trap, and during the addition, internal temperature of the flask was maintained at 140 to 149 C. The resulting reaction mixture was a mixed composition containing the compounds general formulae (7) to (10), and analysis by gas chromatography confirmed that weight ratio of the compounds of formulae (7) to (10), namely, the compound of the formula (7):the compound of the formula (8):the compound of the formula (9):the compound of the formula (10) in the mixed composition was 71:6:4:19. The reaction mixture was distilled to obtain 68 g of a fraction having a boiling point of 140 to 141 C. at 0.4 kPa.The thus obtained fraction was evaluated by mass spectrum, 1H-NMR spectrum (deuterated chloroform solvent), and IR spectrum. The results confirmed that the resulting compound was 1,1-dimethoxy-3-(4-methylpiperadino)methyl-2,5-dioxa-1-silacyclooctane, and the yield in terms of silicon was 75%.
  • 51
  • [ 109-01-3 ]
  • [ 2530-83-8 ]
  • [ 1222257-17-1 ]
  • [ 1222257-23-9 ]
  • [ 1222257-21-7 ]
YieldReaction ConditionsOperation in experiment
84% With sodium methylate; In methanol; toluene;Reflux;Product distribution / selectivity; The procedure of Example 9 was repeated except that 1.5 g of solution of sodium methoxide in methanol (28% by weight of sodium methoxide) was added to the flask during the reaction. The resulting reaction mixture was a mixed composition containing the compounds general formulae (7) to (10), and analysis by gas chromatography confirmed that weight ratio of the compounds of formulae (7) to (10), namely, the compound of the formula (7):the compound of the formula (8):the compound of the formula (9):the compound of the formula (10) in the mixed composition was 68:2:6:24. The reaction mixture was distilled to obtain 102 g of a fraction having a boiling point of 140 to 141 C. at 0.4 kPa.The thus obtained fraction was evaluated by mass spectrum, 1H-NMR spectrum (deuterated chloroform solvent), and IR spectrum. The results confirmed that the resulting compound was 1,1-dimethoxy-3-(4-methylpiperadino)methyl-2,5-dioxa-1-silacyclooctane, and the yield in terms of silicon was 84%.
  • 52
  • [ 1438-82-0 ]
  • [ 2530-83-8 ]
  • [ 1242030-61-0 ]
  • [ 1242030-62-1 ]
  • 53
  • [ 2052-01-9 ]
  • [ 2530-83-8 ]
  • [ 1226791-25-8 ]
  • 54
  • [ 1254067-29-2 ]
  • [ 2530-83-8 ]
  • [ 1254067-30-5 ]
  • 55
  • [ 1438-82-0 ]
  • [ 2530-83-8 ]
  • [ 1242030-61-0 ]
  • [ 1242030-62-1 ]
  • C13H32O6Si3 [ No CAS ]
  • 56
  • [ 109-01-3 ]
  • [ 2530-83-8 ]
  • [ 1222257-17-1 ]
YieldReaction ConditionsOperation in experiment
In chloroform; at 85 - 95℃; for 6h;Reflux; Synthesis Example 1 Synthesis of 2,2-dimethoxy-8-(4-methylpiperazinyl)methyl-1,6-dioxa-2-silacyclooctane A flask equipped with a stirrer, reflux condenser, dropping funnel and thermometer was charged with 30 g (0.30 mol) of methylpiperazine. With stirring at 85-95C, 71 g (0.30 mol) of gamma-glycidoxypropyltrimethoxysilane was added dropwise over 4 hours. Stirring was continued for 2 hours at the temperature, obtaining a clear reaction solution. On distillation of the reaction solution, 39 g of a clear fraction at a boiling point of 140-142C/0.4 kPa was collected. The fraction was analyzed by mass spectrometry, 1H-NMR (in heavy chloroform), and IR spectroscopy. The data of mass spectrometry are given below. m/z 304, 273, 34, 139, 113
  • 57
  • [ 1215088-66-6 ]
  • [ 2530-83-8 ]
  • [ 1286630-52-1 ]
  • 58
  • [ 1286630-51-0 ]
  • [ 2530-83-8 ]
  • [ 1286630-55-4 ]
  • 59
  • [ 288-88-0 ]
  • [ 2530-83-8 ]
  • C11H23N3O5Si [ No CAS ]
  • 60
  • [ 61-82-5 ]
  • [ 2530-83-8 ]
  • [ 1263572-27-5 ]
  • 61
  • [ 124-22-1 ]
  • [ 2530-83-8 ]
  • [ 932748-88-4 ]
YieldReaction ConditionsOperation in experiment
In tetrahydrofuran; at 58℃; for 48h;Inert atmosphere; 5-(4-Carboxyphenyl)-10,15,20-tris(4-methylphenyl)porphyrin (P-acid) was synthesized as previously described.23 The synthesis of the films based on bridged silsesquioxane was reported before.24 The precursor of the silsesquioxane was synthesized employing stoichiometric amounts of DA and GPTMS. The reaction was carried out in 0.4 M THF solution at 58 C for 48 h under nitrogen atmosphere, attaining complete conversion. The hydrolysis and condensation was performed at room temperature, employing 0.1 M solutions in THF adding an appropriate amount of water and catalyst (formic acid) in order to obtain the molar ratio Si/HCOOH/H2O = 1/0.1/3. Solutions (25 mL) were cast in polyacetal recipients of 5 cm diameter with an initial height of liquid of close to 5 mm and place in an oven at 30 C for 24 h. Hydrolysis and condensation reactions took place together with solvent evaporation. Films doped with porphyrin were synthesis as follow: after adding the reactants for hydrolysis and condensation, the corresponding amount of porphyrin was incorporated from a 4 × 10-4 M P-acid stock solution in THF. The porphyrin concentration was checked by spectroscopy, taking into account the value of molar extinction coefficients (epsilon); P-acid epsilon = 4.05 × 105 M-1 cm-1 at 424 nm in THF.25 The mixture was placed in the polyacetal recipients until complete solvent evaporation. Three kinds of films were synthesized, film A: undoped (SSO); film B: doped with 8.8 × 10-6 M P-acid (SSO-P) and film C: doped with 1.8 × 10-5 M P-acid. These concentrations were calculated with all the reactants before hydrolysis and polycondensation of the films take place.
  • 62
  • [ 627-37-2 ]
  • [ 2530-83-8 ]
  • [ 1418032-09-3 ]
YieldReaction ConditionsOperation in experiment
at 50℃; 10 mol of <strong>[2530-83-8]3-glycidoxypropyltrimethoxysilane</strong> (KBM-403 manufactured by Shinetsu, Co., Ltd.) was diluted in propylene glycol monomethyl ether acetate. The solution was maintained at 50 C., and the reaction was performed while 10 mol of N-methylallylamine (Aldrich) was slowly added. After the obtained solution was separated through the column, the solvent was removed by using the vacuum distillation to obtain the compound represented by the following Formula 5.10080]
  • 63
  • [ 2530-83-8 ]
  • [ 1448363-56-1 ]
  • [ 1448363-57-2 ]
  • [ 1448363-61-8 ]
  • [ 1448363-59-4 ]
  • [ 1448363-62-9 ]
  • [ 189232-82-4 ]
  • [ 1448363-54-9 ]
  • [ 1448363-53-8 ]
  • [ 1448363-52-7 ]
  • [ 90052-37-2 ]
  • [ 39006-72-9 ]
  • 64
  • [ 2530-83-8 ]
  • [ 1448363-56-1 ]
  • [ 1448363-64-1 ]
  • [ 1448363-65-2 ]
  • [ 1448363-68-5 ]
  • [ 90052-37-2 ]
  • 65
  • [ 2530-83-8 ]
  • [ 1448363-56-1 ]
  • [ 1448363-64-1 ]
  • [ 1448363-65-2 ]
  • [ 90052-37-2 ]
  • C6H14O5Si [ No CAS ]
  • 66
  • [ 2530-83-8 ]
  • [ 1448363-56-1 ]
  • [ 1448363-64-1 ]
  • [ 1448363-68-5 ]
  • [ 90052-37-2 ]
  • C6H14O5Si [ No CAS ]
  • 67
  • [ 2530-83-8 ]
  • [ 1448363-56-1 ]
  • [ 1448363-64-1 ]
  • [ 1448363-68-5 ]
  • [ 90052-37-2 ]
  • 68
  • [ 2530-83-8 ]
  • [ 1448363-61-8 ]
  • [ 1448363-59-4 ]
  • [ 189232-82-4 ]
  • [ 1448363-54-9 ]
  • [ 1448363-53-8 ]
  • [ 39006-72-9 ]
  • 69
  • [ 2530-83-8 ]
  • [ 189232-82-4 ]
  • [ 1448363-66-3 ]
  • [ 1448363-54-9 ]
  • [ 1448363-53-8 ]
  • [ 1448363-52-7 ]
  • [ 90052-37-2 ]
  • [ 39006-72-9 ]
  • 70
  • [ 2530-83-8 ]
  • C6H14O5Si [ No CAS ]
  • C7H16O5Si [ No CAS ]
  • C8H18O5Si [ No CAS ]
  • 71
  • [ 78-10-4 ]
  • [ 2530-83-8 ]
  • silica [ No CAS ]
YieldReaction ConditionsOperation in experiment
Alkoxysilanes suitable for the invention may include the following compounds: tetramethoxysilane (written TMOS), tetraethoxysilane (written TEOS), tetra-n-propoxysilane,methyltrimethoxysilane, methyltriethoxysilane, ethyltrimethoxysilane, ethyltriethoxysilane, propyltrimethoxysilane, propyltriethoxysilane, isobutyltrimethoxysilane, isobutyltriethoxysilane, octyltrimethoxysilane, octyltriethoxysilane, hexadecyltrimethoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane,3-(trimethoxysilyl)propyl methacrylate, 3-(trimethoxysilyl)propyl acrylate, 3-(trimethoxysilyl)methyl methacrylate, 3-(trimethoxysilyl)methyl acrylate, 3-(trimethoxysilyl)ethyl methacrylate, 3-(trimethoxysilyl)ethyl acrylate, 3-(trimethoxysilyl)pentyl methacrylate, 3-(trimethoxysilyl)pentyl acrylate, 3-(trimethoxysilyl)hexyl methacrylate, 3-(trimethoxysilyl)hexyl acrylate, 3-(trimethoxysilyl)butyl methacrylate, 3-(trimethoxysilyl)butyl acrylate, 3-(trimethoxysilyl)heptyl methacrylate, 3-(trimethoxysilyl)heptyl acrylate, 3-(trimethoxysilyl)octyl methacrylate, 3-(trimethoxysilyl)octyl acrylate,3-glycidyloxypropyltrimethoxysilane, 3-glycidyloxypropyltriethoxysilane,3-methacryloyloxypropyltrimethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, 3-mercaptopropyltrimethoxysilane,3-aminopropyltriethoxysilane, 3-aminopropyltrimethoxysilane, 2-amino'thyl-3-aminopropyltrimethoxysilane, N-(n-butyl)-3-aminopropyltrimethoxysilane.
LIST OF ACRONYMSAPTES Aminopropyl triethoxysilaneDMF DimethylformamideEPI EpichlorohydrinGPTS Glycidoxypropyl trimethoxysilaneHMDI Hexamethylene diisocyanate
  • 73
  • [ 2530-83-8 ]
  • [ 7585-39-9 ]
  • C50H88O40Si [ No CAS ]
  • 74
  • [ 1173883-99-2 ]
  • [ 2530-83-8 ]
  • C32H36N4O9Si [ No CAS ]
  • 75
  • [ 2530-83-8 ]
  • [ 107-15-3 ]
  • [ 482617-82-3 ]
  • 77
  • [ 2530-83-8 ]
  • [ 10016-20-3 ]
  • C45H80O35Si [ No CAS ]
  • 78
  • [ 3345-50-4 ]
  • [ 2530-83-8 ]
  • KH560-NCM [ No CAS ]
  • 79
  • [ 110-91-8 ]
  • [ 2530-83-8 ]
  • [ 1222257-40-0 ]
YieldReaction ConditionsOperation in experiment
In methanol; at 80℃; for 5h;Inert atmosphere; Reflux; (0184) In a round-bottom flask, 28.36 g (120 mmol) of <strong>[2530-83-8]3-glycidoxypropyltrimethoxysilane</strong> (Dynasylan GLYMO from Evonik Degussa), 12.55 g (144.1 mmol) of anhydrous morpholine and 7.00 g of anhydrous methanol were stirred under a nitrogen atmosphere and under reflux at 80 C. over the course of 5 h until no further reaction progress was found by means of gas chromatography. The crude product was aftertreated at 80 C. and about 1 mbar over the course of 30 minutes. A liquid product having a theoretical OH equivalent weight of 323.5 g was obtained. (0185) The reaction product had a purity of 76% by weight after the preparation and a purity of 52% by weight after storage with exclusion of moisture at room temperature for 1 month (determined by means of gas chromatography).
  • 80
  • [ 2494-89-5 ]
  • [ 2530-83-8 ]
  • C17H31NO11S2Si [ No CAS ]
YieldReaction ConditionsOperation in experiment
With formic acid; In N,N-dimethyl-formamide; at 80℃; for 8h; Weighed 2.5g of ([beta] sulfate ethylsulfonyl) aniline, was added to the 30gN, N- dimethyl formamide,Put on a magnetic stirrer, stirred to dissolve.([beta] sulfate ethylsulfonyl) aniline was completely dissolved, the solution thereto was added to 100ml three-necked flask,that began to heat up until the temperature reached to 80 deg C, 1.8ggamma- (2,3- epoxypropoxy) propyl trimethoxysilane and 0.33ml of formic acid were added, the reaction began. Obtained after 8h gamma- (2,3- epoxypropoxy) propyl trimethoxysilane and right ([beta] sulfate ethylsulfonyl) benzene Amine reaction product.
  • 81
  • [ 2530-83-8 ]
  • [ 115-19-5 ]
  • C13H24O5Si [ No CAS ]
YieldReaction ConditionsOperation in experiment
26.4 g With potassium carbonate; at 90℃; for 24h;Inert atmosphere; Reflux; In 250ml three equipped with a magnetic sub, reflux condenser, and nitrogen bubbler means round-bottomed flask were added successively 25.3g (0.3mol) methylbutynol, 23.6g (0.1mol) (2,3- ring oxygen propoxy) propyl trimethoxy silane, 0.1g of potassium carbonate. 90 degrees for 24 hours. After the reaction was cooled and filtered to remove potassium carbonate. Removing low boiling point of the pump 150, to give a colorless transparent liquid 26.4g.
  • 82
  • [ 2530-83-8 ]
  • [ 110-70-3 ]
  • C22H52N2O10Si2 [ No CAS ]
YieldReaction ConditionsOperation in experiment
With propylene glycol methyl ether acetate; at 50℃; N, N'-dimethylethylenediamine (Aldrich) 10mol and, <strong>[2530-83-8]3-glycidoxypropyltrimethoxysilane</strong> The (Shinetsu KBM-403) 20mol, Each was diluted with propylene glycol monomethyl ether acetate. N, N'- dimethylethylenediamine has been diluted solution was maintained at 50 , <strong>[2530-83-8]3-glycidoxypropyltrimethoxysilane</strong> (Shinetsu KBM-403) slowly a solution diluted is It was added and allowed to react. The resulting solution was separated by column, Using a vacuum distillation to remove the solvent, To give a compound represented by the chemical formula 3.
  • 83
  • [ 2530-83-8 ]
  • C9H21N3O5Si [ No CAS ]
  • 84
  • [ 2530-83-8 ]
  • [ 6898-84-6 ]
  • C11H24O4SSi [ No CAS ]
  • C12H28O5SSi [ No CAS ]
  • 85
  • [ 124-41-4 ]
  • [ 2530-83-8 ]
  • C10H24O6Si [ No CAS ]
Same Skeleton Products
Historical Records

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[ 2530-83-8 ]

Organosilicon

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[ 2602-34-8 ]

Triethoxy(3-(oxiran-2-ylmethoxy)propyl)silane

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Trimethoxy(3-methoxypropyl)silane

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