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CAS No. : | 17875-55-7 | MDL No. : | MFCD00411646 |
Formula : | C16H24O2Si3 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | BSXVSQHDSNEHCJ-UHFFFAOYSA-N |
M.W : | 332.62 | Pubchem ID : | 6335362 |
Synonyms : |
|
Num. heavy atoms : | 21 |
Num. arom. heavy atoms : | 12 |
Fraction Csp3 : | 0.25 |
Num. rotatable bonds : | 6 |
Num. H-bond acceptors : | 2.0 |
Num. H-bond donors : | 0.0 |
Molar Refractivity : | 97.83 |
TPSA : | 18.46 Ų |
GI absorption : | High |
BBB permeant : | Yes |
P-gp substrate : | No |
CYP1A2 inhibitor : | Yes |
CYP2C19 inhibitor : | No |
CYP2C9 inhibitor : | No |
CYP2D6 inhibitor : | Yes |
CYP3A4 inhibitor : | No |
Log Kp (skin permeation) : | -4.38 cm/s |
Log Po/w (iLOGP) : | 3.93 |
Log Po/w (XLOGP3) : | 5.56 |
Log Po/w (WLOGP) : | 2.24 |
Log Po/w (MLOGP) : | 2.92 |
Log Po/w (SILICOS-IT) : | -0.22 |
Consensus Log Po/w : | 2.89 |
Lipinski : | 0.0 |
Ghose : | None |
Veber : | 0.0 |
Egan : | 0.0 |
Muegge : | 1.0 |
Bioavailability Score : | 0.55 |
Log S (ESOL) : | -5.43 |
Solubility : | 0.00123 mg/ml ; 0.0000037 mol/l |
Class : | Moderately soluble |
Log S (Ali) : | -5.71 |
Solubility : | 0.000651 mg/ml ; 0.00000196 mol/l |
Class : | Moderately soluble |
Log S (SILICOS-IT) : | -6.23 |
Solubility : | 0.000197 mg/ml ; 0.000000593 mol/l |
Class : | Poorly soluble |
PAINS : | 0.0 alert |
Brenk : | 1.0 alert |
Leadlikeness : | 1.0 |
Synthetic accessibility : | 4.59 |
Signal Word: | Danger | Class: | 9 |
Precautionary Statements: | P273-P201-P264-P280-P301+P330+P331-P312 | UN#: | 3082 |
Hazard Statements: | H302-H361-H372-H410 | Packing Group: | Ⅲ |
GHS Pictogram: |
* 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.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With platinum |
Yield | Reaction Conditions | Operation in experiment |
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With water |
Yield | Reaction Conditions | Operation in experiment |
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In hexane |
Yield | Reaction Conditions | Operation in experiment |
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60.6% | With dihydrogen hexachloroplatinate at 80℃; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
80.7% | at 120℃; for 8h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
80% | With water at 20℃; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 1: 60.6 percent / H2PtCl6 / 80 °C 2: 69.3 percent / H2PtCl6 / 80 °C |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
98.7% | In toluene at 80 - 120℃; for 2h; | 2 A four-neck flask equipped with a stirrer was filled with 287.4 g (0.86 mol) of l,l,555-tetramethyl-3,3-diphenyltrisiloxane, 160 g of toluene, and 0.06 g of a platinum- 1,3- divinyl-l,l,3,3-tetramethyldisiloxane complex (concentration of metal platinum was 4 wt.%). The contents were heated to 80°C, and 312.6 g (1.90 mol) of eugenol were added dropwise. A reaction was carried out for 2 hours at 1200C. After the reaction mixture was stripped under a reduced pressure, 564 g of a brown transparent liquid having a viscosity of 2,700 mPa-s were produced with yield of 98.7%. 13C-NMR and 29Si-NMR analyses showed that the product was an organotrisiloxane represented by the following formula: |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
96.8% | In toluene at 80 - 120℃; for 2h; | 1 A four-neck flask equipped with a stirrer was filled with 81.3 g (0.24 mol) of l,l,5,5-tetramethyl-3,3-diphenyltrisiloxane, 100 g of toluene, and 0.025 g of a platinum- l,3-divinyl-l,l,3,3-tetramethyldisiloxane complex (concentration of metal platinum was 4 wt.%). The contents were heated to 8O0C, and 79.1 g (0.59 mol) of 2-allylphenol were added dropwise. A reaction was carried out for 2 hours at 12O0C. After the reaction mixture was stripped under a reduced pressure, 142.6 g of a brown liquid having a EPO viscosity of 3,500 niPa-s were produced with yield of 96.8%. 13 C/ -Nuclear Magnetic Resonance Analysis (hereinafter referred to as NMR analysis) and 29Si-NMR analysis showed that the product was an organotrisiloxane represented by the following formula: |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
13.6 g | Stage #1: diphenylsilanediol With tris(pentafluorophenyl)borate In 5,5-dimethyl-1,3-cyclohexadiene at 40℃; Inert atmosphere; Stage #2: 1,1,5,5-tetramethyl-3,3-diphenyl-trisiloxane In 5,5-dimethyl-1,3-cyclohexadiene at 40 - 60℃; for 2h; Inert atmosphere; | 7 Example 7 Synthesis of 1,1,5,5-Tetraphenyl-3,3,7,7-tetramethylcyclotetrasiloxane (“Tetraphenyl-D4”) In a dry 100 L round bottom flask fitted with a magnetic stirrer, condenser, thermocouple probe with temperature control, heating mantle and nitrogen over-gas was placed 13 g (0.06 mole) DPSD and 30 g xylenes. The mixture was heated to 40° C. and stirred to dissolve the DPSD. Using a syringe, 0.2 ml of a 5% tris(pentafluorophenyl)boron in xylenes was added to yield a boron complex concentration of 150 ppm in the solution. From an addition funnel was added 22.2 g (0.06 mole) 3,3-Diphenyl-1,1,5,5-tetramethyltrisiloxane (M′, DPh2M′) at a rate that maintained a slow steady evolution of hydrogen gas. The addition continued for about 1 hour at 40-60° C. Once addition was completed, the reaction mixture was stirred at 60° C. for an hour. When an FTIR analysis of the reaction mixture displayed no signal for SiH at ˜2150 cm-1 and a GC analysis showed about a 79% yield of Tetraphenyl-D4, 0.1 g of magnesium oxide was added to neutralize the catalyst and the reaction mixture was stirred for 30 minutes. The mixture was filtered into a 100 ml round bottom flask and the solvent was removed using a rotary evaporator at 90° C. and 1H NMR analysis. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
94% | With platinum(0)-1,3-divinyl-1,1,3,3-tetramethyldisiloxane complex In toluene at 60 - 80℃; for 1.16667h; | 5 Example 5: Preparation of H-4 To a stirred mixture of 5 grams (0.01 4mol) of S- 1 prepared in examplel, 10 grams of toluene and platinum catalyst shown by Karstedt, U.S. Pat. No. 3,775,452 (i.e., Platinate(2-), hexachloro-, dihydrogen, (OC-6- 11)-, reaction products with 2,4,6,8 -tetraethenyl-2 ,4,6,8- tetramethylcyclotetrasiloxane was used), to provide 5 ppm of Pt catalyst based on a total amount of S-i and hydrogen siloxane at 60°C was added 4.6 grams (0.01 4mol) of l,l,i-triphenyl-3,3- dimethyldisiloxane over a period of 10 minutes. An exotherm was observed during the addition to about 80°C. After complete addition, the mixture was stirred for an additional 1 how at 80°C to complete a hydrosilylation reaction. The toluene solution was then heated to 120°C and stripped at reduced pressure to remove the toluene, leaving 9 grams (94% of theory) of a white crystalline product with n25/D=l .536 in 50% toluene solution and a melting point of 95-99°C. This product was identified as H-I by 1H-NMR analysis.A procedure similar to Example 2 was performed, except that 4.4 grams (0.Ol3mol) of a hydrogen siloxane was used having a fonnula of Ph2Si[OS1Me2H]2 (wherein Ph is phenyl and Me is methyl), 10 grams (0.028mo1) of 5-1. There was obtained 13.5 grams (94% of theory) of a white crystalline product with n25/D= 1.528 in 50% toluene solution and a melting point of 60- 65°C. This product was identified as H-4 by I H-NMR analysis. |
94% | With dihydrogen hexachloroplatinate In toluene at 60 - 80℃; for 1.16667h; | 5 Example 5: Preparation of Silicone H-4-‘ A procedure simikir to Example 2 was perfbrmect except that 4.4 gnims (0.013 mole) of a silvi hydridccontaining compound having a thnnu]a of Pb2Si[OSiMC2.H]2 (wherein Ph is phenyl and Me is methyl) and 10 grams (0.028 mole) of S-I i’here was obtained 13.5 grams (94% of theory) of a white crystalline product with a refractive index measured at 25 C of 1.528 in 50% (oluene solution and a melting point of 60-65T. This product was identified as 1-1-4 by 1H-NMR analysis. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
98% | In acetonitrile at 20℃; for 0.5h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With platinum catalyst; In toluene; at 119 - 130℃; for 48h; | (1) taking 0.5 g of hydrosilylation catalyst platinum, diluted with 5 mL of toluene, and then added to a 250 mL three-necked flask; (2) 2.49g of 1,3,5-Triallyl-1,3,5-triazine-2,4,6(1H,3H,5H)-trione (1,3,5-Triallyl-1) , 3,5-triazine-2,4,6(1H,3H,5H)-trione, molecular weight MW=249.27g/mol),diluted with 20mL of toluene and added to a three-necked flask; (3) Take 15.00g of 1,1,5,5-tetramethyl-3,3-diphenyltrisiloxane (1,1,5,5-tetramethyl-3,3-diphenyltrisiloxane, molecular weight = 333) Diluted with 25 mL of toluene and added to a three-necked flask; (4) Set the oil bath temperature to 130 C, turn on the stirring, and turn on the condensed water. When the temperature in the three-necked flask is 119 C, the reaction mixture starts to reflux; (5) After refluxing for a while, a small amount of the reaction mixture is taken for IR test to determine whether the reaction is complete. (6) After 48 hours, the IR results showed that the carbon-free carbon double bond absorption peak indicates the end of the reaction, and the 1H NMR results showed no vinyl H. At this time, the reaction mixture was transferred to a rotary evaporator to distill off the solvent, and the product cross-linking agent was precipitated. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With hexachloroplatinic acid at 80℃; for 3h; | 5 Example 3 The aqueous solution of benzyl triethylammonium chloride (a concentration of 1500g / L, 20mL) and halloysite nanotube (50g) mixing, in addition to the dry water by evaporation, the remaining material placed in a heating ultrasonic microwave apparatus 180 15min, to give a solid containing benzyl triethyl ammonium chloride halloysite nanotube catalyst. Eugenol was added under atmospheric pressure and epichlorohydrin (mole ratio 1: 1), prepared according to the present embodiment contains a proportion of solids added benzyltriethylammonium chloride as catalyst halloysite nanotube (benzyl the molar ratio of eugenol triethylammonium chloride = 0.05: 1), ring-opening etherification reaction is carried out at 120 °C, the reaction time was 4 hours, to give chlorohydrin ether; be cooled to about 60°C system to the system sodium hydroxide was added (molar ratio of sodium hydroxide to eugenol = 1.05: 1), added portionwise over 3 hours, holding for 10 hours, the organic phase obtained is the product of an epoxy of eugenol. Yield (calculated by a phenolic hydroxy compound) was 95%. After testing, epoxidized eugenol prepared in the present embodiment the hydrolyzable chlorine content of 60ppm, inorganic chlorine content was 3ppm. A hydrosilylation reaction with 1,1,5,5-tetramethyl-3,3-diphenyl-trisiloxane the epoxidation eugenol chlorination platinic acid (30 ppm or) at 80°C (molar ratio of epoxidized eugenol 1,1,5,5-tetramethyl trisiloxane 3,3-diphenyl-2: 1), the reaction time was 3 hours, the reaction was completed to obtain eugenol epoxy resin. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Stage #1: 4-allylguaiacol; epichlorohydrin at 120℃; for 4h; Stage #2: 1,1,5,5-tetramethyl-3,3-diphenyl-trisiloxane With dihydrogen hexachloroplatinate at 80℃; for 3h; | 5 0.1 mol of benzyldiethylamine, 0.1 mol of γ-chloropropyltriethoxysilane, 200 mL of ethanol, 0.05 mol ofpotassium iodide, heated to 70 ° C under nitrogen atmosphere, reacted for 2 hours, and the product wasfiltered to obtain a quaternary ammonium salt mother liquor. 100 mL of quaternary ammonium salt was added to 120 mL of distilled water/ethanol (40 ml of water, 80 ml of ethanol), and the pH of the solution was adjusted to4.5 with glacial acetic acid. After standing for 3 hours, 60 g of halloysite nanotubes were placed therein. After fullyimmersing for 2.5 hours, the water is removed by evaporation, and the obtained product is a quaternaryammonium salt functionalized halloysite nanotube. Eugenol and epichlorohydrin (molar ratio 1:1) were added under normal pressure, and the quaternaryammonium salt functionalized halloysite nanotubes prepared in this example were added as a catalyst(benzyltriethylammonium chloride). The molar ratio of eugenol to 0.05:1), etherification ring-opening reactionat 120 ° C, the reaction time is 4 hours, to obtain chlorohydrin ether; to cool the system to about 60 ° C to addsodium hydroxide to the system (Molar ratio of sodium hydroxide to eugenol = 1.05:1), added in batches within3 hours, and the reaction was kept for 10 hours; the system was allowed to stand for cooling and layering, and theobtained organic phase product was epoxidized eugenol. The yield (calculated as phenolic hydroxyl compound)was 95%. The epoxidized eugenol prepared in the present example was tested to have a hydrolyzable chlorinecontent of 60 ppm and an inorganic chlorine content of 3 ppm. to 120 mL of distilled water/ethanol (40 ml of water, 80 ml of ethanol), and the pH of the solution was adjusted to4.5 with glacial acetic acid. After standing for 3 hours, 60 g of halloysite nanotubes were placed therein. After fullyimmersing for 2.5 hours, the water is removed by evaporation, and the obtained product is a quaternaryammonium salt functionalized halloysite nanotube. Eugenol and epichlorohydrin (molar ratio 1:1) were added under normal pressure, and the quaternaryammonium salt functionalized halloysite nanotubes prepared in this example were added as a catalyst(benzyltriethylammonium chloride). The molar ratio of eugenol to 0.05:1), etherification ring-opening reactionat 120 ° C, the reaction time is 4 hours, to obtain chlorohydrin ether; to cool the system to about 60 ° C to addsodium hydroxide to the system (Molar ratio of sodium hydroxide to eugenol = 1.05:1), added in batches within3 hours, and the reaction was kept for 10 hours; the system was allowed to stand for cooling and layering, and theobtained organic phase product was epoxidized eugenol. The yield (calculated as phenolic hydroxyl compound)was 95%. The epoxidized eugenol prepared in the present example was tested to have a hydrolyzable chlorinecontent of 60 ppm and an inorganic chlorine content of 3 ppm. Chloroplatinic acid (30 ppm) was added to epoxidized eugenol, and hydrosilylation reaction with 1,1,5,5-tetramethyl-3,3-diphenyltrisiloxane was carried out at 80 °C. (The molar ratio of epoxidized eugenol to 1,1,5,5-tetramethyl-3,3-diphenyltrisiloxane is 2:1), the reaction time is 3 hours, and the reaction is completed to obtainthe organism. Base epoxy resin. It can be seen from the nuclear magnetic test that the structural formula of the bio-based epoxy resin prepared inthis embodiment is as shown in (I-3). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
88.97% | Add 200 g of <strong>[6843-66-9]<strong>[6843-66-9]diphenyldimethoxysilan</strong>e</strong> to a 2 L four-necked flask equipped with a thermometer, a constant pressure dropping funnel, a stirrer, and a condenser. Then, add 20 g of concentrated sulfuric acid having a mass concentration of 98%, and mix for 10 minutes. The constant pressure dropping funnel was slowly added dropwise 400 g of tetramethyldihydrodisiloxane, and the addition time was 4 h. After the completion of the dropwise addition, stirring was continued for 24 hours, 80 g of sodium carbonate was added for neutralization for 2 hours, vacuum filtration was carried out, and the filtrate was distilled under reduced pressure. A fraction of 130 to 131 C / 2.5 mmHg was taken to obtain a colorless transparent liquid, which was tetramethyldihydrodiphenyltrisiloxane. The weight was 242 g, the yield was 88.97%, and the chromatographic detection content was 99.5%. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
70 g | With platinum catalyst In toluene at 70℃; Inert atmosphere; | 1.1-1.3 (1) In a N2 atmosphere, add 300 g of toluene to a three-necked 1000 mL flask equipped with a thermometer and a condenser, and then add 17.23 g of 2,4,6,8-tetravinyl-2,4,6,8-tetramethyl Cyclotetrasiloxane (CAS No. 2554-06-5, 2,4,6,8-Tetravinyl-2,4,6,8-tetramethylcyclotetrasiloxane) and 0.44g platinum catalyst, heated to 70 and stirred with a magnetic stirrer .(2) Pass 33.26g of 1,1,5,5-tetramethyl-3,3-diphenyltrisiloxane through a 100mL pressure balance feeding funnel(CAS No. 17875-55-7, 1,1,5,5-Tetramethyl-3,3-diphenyltrisiloxane)And 24.05g of 2,4,6,8-tetramethylcyclotetrasiloxane (CAS No. 2370-88-9, 2,4,6,8-Tetramethylcyclotetrasiloxane) was added dropwise to the obtained in step (1) In the mixture, the dripping is completed within 0.5-1.0h, and then the reaction is continued for 12h. The reaction temperature in the flask fluctuates from 69°C to 80-90°C. The reaction process is monitored by FT-IR and NMR spectroscopy. The reaction is terminated after the Vi functionality disappears.(3) Transfer the final mixed reactant obtained in step (2) to a 1L single-neck flask, and use a rotary evaporator to extract toluene under high vacuum conditions, and finally obtain about 72g of colorless oil, which is the target product. The characterization data of 1H NMR, 13C NMR, FT-IR (see also Figure 1) are as follows: |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
99% | With tetramethyldivinyldisiloxane at 140℃; for 0.5h; | 1 167.2 g of vinylcyclohexenoxide was placed in a 500 ml three-necked round-bottom flask equipped with a reflux tube, a dropping funnel, and a thermometer, and 42 mg of a divinyltetramethyldisiloxane solution of a divinyltetramethyldisiloxane complex having a platinum content of 4% was added. Add and heat while stirring with a magnetic stirrer, stop heating at 140 ° C, and add 21,9.5 g of 1,1,5,5-tetramethyl-3,3-diphenyl-trisiloxane while maintaining 140 ° C. It was dropped slowly. An exothermic reaction occurred during the dropping, and the temperature could be maintained without heating. After completion of the dropping, the mixture was heated and maintained at 140 ° C. for 30 minutes, and excess vinylcyclohexene oxide was distilled off under reduced pressure. A yield of 197 g was obtained. This was a 99% yield with respect to the dropped 1,1,5,5-tetramethyl-3,3-diphenyl-trisiloxane. The refractive index was 1.5200 and the measured epoxy equivalent was 300. The theoretical value of epoxy equivalent is 291. The 1,5-bis (β- (3,4-epoxycyclohexyl) ethyl) -1,1,5,5-tetramethyl-3,3-diphenyl-trisiloxane of the present invention has high reactivity and high refractive index. It has good compatibility with various epoxy resins and is useful as a siloxane-modifying material for various epoxy resins. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With tris(pentafluorophenyl)borate In toluene at 70℃; for 7.5h; | 1 In a four-necked flask equipped with a stirrer, a cooling pipe, a dropping funnel and a thermometer, Trispentafluorophenylboran 0.3 g (5.9 x 10-4 mol), Was added and dissolved in 100 g of toluene. Add 33.3 g (0.40 mol) of 2-methyl-3-butyne-2-ol to this. In addition, the temperature was raised to 70 ° C. To this, 60.0 g (0.18 mol) of the compound represented by the following formula (A) was added dropwise over 30 minutes using a dropping funnel. After completion of the dropping, the mixture was further heated and stirred at 70 ° C. for 7 hours. After heating, cool to room temperature (25 ° C) , Magnesium / Aluminum to adsorb and remove the trispentafluorophenylborane 3 g of a nium-based solid solution (commodity: KW-2200, manufactured by Kyowa Chemical Industry Co., Ltd.) was added, and the mixture was stirred at room temperature for 1 hour. KW-2200 was removed by pressure filtration, and the residual solvent was distilled off by reducing the pressure to obtain an alkynyl group-containing organopolysiloxane (Compound 1) represented by the following formula (B). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 1: platinum on activated charcoal / ethyl acetate / 4 h / 80 °C / Inert atmosphere 2: triethylamine / dichloromethane / 0 °C |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With platinum on activated charcoal In ethyl acetate at 80℃; for 4h; Inert atmosphere; | 2 Preparative Example 2: Preparative Example 2: Preparation of Silicone Based Di(Meth)Acrylate In a 1,000 ml flask provided with a cooling tube and a stirrer, 300 ml of ethyl acetate, 21 g of 3,3-diphenyl-1,1,5,5-tetramethyltrisiloxane and 43 g of allyl alcohol (Daejung Chemicals & Materials Co., Ltd.) were placed, followed by nitrogen purging for 30 minutes. Next, 72 ppm of Pt-on-carbon black powder (Aldrich GmbH) was added thereto, followed by heating the flask to 80° C. and stirring the components for 4 hours. The remaining solvent was removed by distillation, thereby obtaining a compound. 71.5 g of the obtained compound and 39 g of triethylamine were sequentially added to 300 ml of dichloromethane, followed by slowly adding 30.2 g of methacryloyl chloride while stirring the mixture at 0° C. The remaining solvent was removed by distillation, thereby obtaining a compound (molecular weight: 584.92 g/mol) represented by Formula 4-2 and having a purity of 96% as measured by HPLC. (1H NMR: δ 7.52, m, 6H; δ 7.42, m, 4H; δ 6.25, d, 2H; δ 6.02, dd, 2H; δ 5.82, t, 1H; δ 5.59, d, 2H; δ 3.86, m, 4H; δ 1.52, m, 4H; δ 0.58, m, 4H; δ 0.04, m, 12H) | |
2250 g | With platinum(0)-1,3-divinyl-1,1,3,3-tetramethyldisiloxane complex In ethyl acetate at 80℃; for 4h; Large scale; | 17 Add 900g 1,1,3,3-tetramethyldisiloxane (L003-1), 1200g diphenylsilane diol (L003-2) and 180g p-toluenesulfonic acid into a 15L three-necked flask and stir for 40°C It was then dissolved in 30L of toluene and washed 5 times with deionized water in a separatory funnel. The toluene was removed by rotary evaporation to obtain 1500 g of compound 1,1,5,5-tetramethyl-3,3-diphenyltrisiloxane (L003-3) with a yield of 81%. Dissolve 1500g of 1,1,5,5-tetramethyl-3,3-diphenyltrisiloxane (L003-3) and 1020g of allyl alcohol (L003-4) in 15L of ethyl acetate and add In the reaction flask, 9 g of the karstedt's catalyst solution containing tetramethyldivinyl disiloxane was added to the reaction system, and the mixture was heated to 80° C. under reflux and stirred for 4 hours. After the temperature was lowered to normal temperature, the Pt catalyst was removed by filtration, and the solvent and residual allyl alcohol were removed by rotary evaporation using a vacuum distillation device to obtain 2250 g of chemical formula L003-5, and 2220 g of isocyanate ethyl acrylate (L003-6) and 9L of toluene was stirred at 50°C for 4 hours after the reaction was completed to obtain compound L002. MW: 731.03. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 1: platinum(0)-1,3-divinyl-1,1,3,3-tetramethyldisiloxane complex / ethyl acetate / 4 h / 80 °C / Large scale 2: toluene / 4 h / 50 °C / Large scale |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 1: platinum(0)-1,3-divinyl-1,1,3,3-tetramethyldisiloxane complex / ethyl acetate / 4 h / 80 °C / Large scale 2: toluene / 4 h / 50 °C / Large scale |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
2400 g | With platinum(0)-1,3-divinyl-1,1,3,3-tetramethyldisiloxane complex In ethyl acetate at 80℃; for 4h; Large scale; | 1 Add 900g of 1,1,3,3-tetramethyldisiloxane (L001-1), 1200g of diphenylsilane diol (L001-2) and 180g of p-toluenesulfonic acid into a 20L reactor and stir for 40°C It was then dissolved in 30L of toluene, separated and washed 5 times with deionized water. The toluene was removed by rotary evaporation to obtain 1476 g of compound 1,1,5,5-tetramethyl-3,3-diphenyltrisiloxane (L001-3) with a yield of 80%. Dissolve 1476g of 1,1,5,5-tetramethyl-3,3-diphenyltrisiloxane (L001-3) and 990g of allylamine (L001-4) in 15L of ethyl acetate and add the reaction In the bottle, 9 g of the karstedt's catalyst solution containing tetramethyldivinyldisiloxane was added to the reaction system, and the mixture was heated to 80° C. under reflux and stirred for 4 hours. After lowering the temperature to normal temperature, filter to remove the Pt catalyst, and use a vacuum distillation device to rotate the solvent and residual allylamine to obtain 2400g of chemical formula L001-5 and 2220g of isocyanate ethyl acrylate (L001-6) and 9L of toluene After stirring at 50°C for 4 hours, the compound L001 can be obtained after the reaction is completed. MW: 727.05. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
2340 g | With platinum(0)-1,3-divinyl-1,1,3,3-tetramethyldisiloxane complex In ethyl acetate at 80℃; for 4h; Large scale; | 9 Add 900g of 1,1,3,3-tetramethyldisiloxane (L002-1), 1200g of diphenylsilane diol (L002-2) and 180g of p-toluenesulfonic acid into a 15L three-necked flask, and stir for 40°C It was then dissolved in 30L of toluene, separated and washed 5 times with deionized water. The toluene was removed by rotary evaporation to obtain 1500 g of compound 1,1,5,5-tetramethyl-3,3-diphenyltrisiloxane (L002-3) with a yield of 81%. Dissolve 1500g of 1,1,5,5-tetramethyl-3,3-diphenyltrisiloxane (L002-3) and 1320g of allyl mercaptan (L002-4) in 15L of ethyl acetate After adding it into the reaction flask, adding 9 g of the karstedt's catalyst solution of tetramethyl divinyl disiloxane into the reaction system, heating to 80° C. under reflux and stirring for 4 hours. After the temperature was lowered to normal temperature, the Pt catalyst was removed by filtration, and the solvent and residual allyl mercaptan were removed by rotary evaporation using a vacuum distillation device to obtain 2340 g of chemical formula L002-5, and 2220 g of isocyanate ethyl acrylate (L002-6). ) And 9L of toluene were stirred at 50°C for 4 hours to obtain compound L002 after the reaction was completed. MW: 763.16. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
81% | With toluene-4-sulfonic acid at 40℃; Large scale; | 1; 9; 17 Add 900g of 1,1,3,3-tetramethyldisiloxane (L002-1), 1200g of diphenylsilane diol (L002-2) and 180g of p-toluenesulfonic acid into a 15L three-necked flask, and stir for 40°C It was then dissolved in 30L of toluene, separated and washed 5 times with deionized water. The toluene was removed by rotary evaporation to obtain 1500 g of compound 1,1,5,5-tetramethyl-3,3-diphenyltrisiloxane (L002-3) with a yield of 81%. Dissolve 1500g of 1,1,5,5-tetramethyl-3,3-diphenyltrisiloxane (L002-3) and 1320g of allyl mercaptan (L002-4) in 15L of ethyl acetate After adding it into the reaction flask, adding 9 g of the karstedt's catalyst solution of tetramethyl divinyl disiloxane into the reaction system, heating to 80° C. under reflux and stirring for 4 hours. After the temperature was lowered to normal temperature, the Pt catalyst was removed by filtration, and the solvent and residual allyl mercaptan were removed by rotary evaporation using a vacuum distillation device to obtain 2340 g of chemical formula L002-5, and 2220 g of isocyanate ethyl acrylate (L002-6). ) And 9L of toluene were stirred at 50°C for 4 hours to obtain compound L002 after the reaction was completed. MW: 763.16. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
93% | at 65℃; for 16h; Inert atmosphere; | 1 Preparation of diethylaminooxy tetramethyl diphenyl trisiloxane Under nitrogen protection, 80g of tetramethyldiphenyldihydrogentrisiloxane (DPHH) was added to the reaction vessel containing 49.31g of N,N-diethylhydroxylamine within 2h,The feeding temperature was kept at about 65°C, and after the feeding was completed, the reaction temperature was kept at 65°C for 16 hours, and the whole reaction was under nitrogen protection.The reacted material was distilled under reduced pressure at 100°C and -0.1MPa for 2h to remove excess N,N-diethylhydroxylamine,The terminal diethylaminooxytetramethyldiphenyltrisiloxane (DPHN) of the above formula can be obtained with a yield of 93%. |
[ 546-56-5 ]
2,2,4,4,6,6,8,8-Octaphenyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocane
Similarity: 0.97