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[ CAS No. 133152-67-7 ] {[proInfo.proName]}

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Chemical Structure| 133152-67-7
Chemical Structure| 133152-67-7
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Product Details of [ 133152-67-7 ]

CAS No. :133152-67-7 MDL No. :N/A
Formula : C18H17F6OSSb Boiling Point : -
Linear Structure Formula :- InChI Key :-
M.W : 517.14 Pubchem ID :-
Synonyms :

Safety of [ 133152-67-7 ]

Signal Word:Danger Class:9
Precautionary Statements:P501-P273-P260-P270-P264-P280-P391-P314-P337+P313-P305+P351+P338-P301+P312+P330 UN#:3077
Hazard Statements:H302-H319-H372-H410 Packing Group:
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Application In Synthesis of [ 133152-67-7 ]

* 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 [ 133152-67-7 ]

[ 133152-67-7 ] Synthesis Path-Downstream   1~7

YieldReaction ConditionsOperation in experiment
82.3% S.3 Synthesis for α-naphthylmethyl-4-hydroxyphenylmethylsulfonium hexafluoroantimonate Synthetic Example 3 Synthesis for α-naphthylmethyl-4-hydroxyphenylmethylsulfonium hexafluoroantimonate α-naphthylmethyl-4-hydroxyphenylmethylsulfonium chloride was dissolved in an amount of 5.00 g (0.015 mol) into 200 ml of methanol, to which 4.08 g (0.015 mol) of powder of KSbF6 was added under stirring. Subsequently, the same procedures as those in Synthesis Example 1 were applied o obtain 6.32 g (82.3% yield) of the aimed product as white crystals. Melting point 125.5°C (decomposition) IR (KBr) cmmin1 3480, 665 NMR (Acetone-d6) ppm δ = 3.57 (3H, S, C H3 S+2 C10H7) δ = 6.93~8.35 (11H, m, -C6 H4 - -CH2C10 H7) δ = 9.72 (1H, S, H O-) Elementary analysis C18H17OSSbF6 Theoretical value C; 41.81%, H; 3.31% Measured value C; 41.63%, H; 3.25%
  • 2
  • [ 133152-67-7 ]
  • [ 133152-87-1 ]
YieldReaction ConditionsOperation in experiment
81% S.15 Synthesis for α-naphthylmethyl-4-(methoxycarbonyloxy)phenylmethylsulfonium hexafluoroantimonate Synthetic Example 15 Synthesis for α-naphthylmethyl-4-(methoxycarbonyloxy)phenylmethylsulfonium hexafluoroantimonate Using α-naphthylmethyl-4-hydroxyphenylmethylsulfonium hexafluoroantimonate synthesised in Synthetic Example 3 as the starting material in an amount of 5.00 g (0.015 mol) and synthesis was conducted in the same procedures as those in Synthetic Example 7 to obtain 6.99 g (81.0% yield) of the aimed product as white crystals. Melting point 125.5~126.0 °C IR (KBr) cmmin1 1760, 1210, 660 NMR (Acetone-d6) ppm δ = 3.65 (3H, s, C H3 S+3 OCOO-) δ = 5.39~5.92 (2H, dd, -C H2 C10H7) δ = 7.33~8.32 (11H, m, -C6 H4 -, -CH2C10 H7) Elementary analysis C20H19O3 SSbF6 Theoretical value C; 41.82%, H; 3.33% Measured value C; 42.12%, H; 3.24%
  • 3
  • [ 133152-67-7 ]
  • [ 133152-89-3 ]
YieldReaction ConditionsOperation in experiment
79.3% S.16 Synthesis for α-naphthylmethyl-4-acetoxyphenylmethylsulfonium hexafluoroantimonate Synthetic Example 16 Synthesis for α-naphthylmethyl-4-acetoxyphenylmethylsulfonium hexafluoroantimonate Using α-naphthylmethyl-4-hydroxyphenylmethylsulfonium hexafluoroantimonate synthesised in Synthetic Example 3 as the starting material in an amount of 5.00 g (0.015 mol) and synthesis was conducted in the same procedures as those in Synthetic Example 7 to obtain 6.65 g (79.3% yield) of the aimed product as white crystals. Melting point 118.0~120.0 °C IR (KBr) cmmin1 1775, 1195, 655 NMR (Acetone-d6) ppm δ = 2.29 (3H, S, C H3 COO-) δ = 3.60 (3H, S, C H3 S+2 C10H7) δ = 7.25~8.31 (11H, m, -C6H4-, -CH2C10 H7) Elementary analysis C20H19O2 SSbF6 Theoretical value C; 43.02%, H; 3.43% Measured value C; 43.19%, H; 3.47%
  • 4
  • [ 2797-28-6 ]
  • [ 133152-67-7 ]
  • 4-hydroxyphenyl(α-naphthylmethyl) methylsulfonium tetrakis(pentafluorophenyl)borate [ No CAS ]
YieldReaction ConditionsOperation in experiment
In water; ethyl acetate for 0.5h; 1 EXAMPLES Examples 1 and 2, Comparative Examples 1 to 4 ; The sulfonium antimonate complexes of the formulae (1d), (1e), and (1f) (refer to Japanese Patent Application Laid-Open No. Hei 10-245378 for the synthesis method) were dissolved in ethyl acetate to prepare respective 10 mass% solutions of such complex in ethyl acetate. Separately, an aqueous solution of 10 mass% of the sodium borate salt of the formula (3) (refer to Japanese Patent Application Laid-Open No. Hei 10-310587 for the synthesis method) was prepared. Next, the aqueous solution of 10 mass% of the sodium borate salt of the formula (3) was mixed at room temperature in an equimolar amount into the 10 mass% solutions of the complexes in ethyl acetate, and the resultant mixtures were stirred as is for 30 minutes. Then, the ethyl acetate layer was separated from the reaction mixtures. The layers were dried, and the ethyl acetate was removed under reduced pressure, whereby the sulfonium borate complex of the formula (1a) of Example 1, the sulfonium borate complex of the formula (1b) of Example 2, and the sulfonium borate complex of (1c) of Comparative Example 1 were obtained as evaporated residues. [Show Image] [Show Image] [Show Image] [Show Image] [Show Image] [Show Image] [Show Image] The novel compound sulfonium borate complexes of the formula (1a) and (1b) were subjected to mass spectroscopy (measuring instrument: ACQUITY UPLC System, Waters), elemental analysis (measuring instrument: PHOENIX, EDAX), IR analysis (measuring instrument: 7000e FT-IR, Varian), and 1H-NMR analysis (measuring instrument: MERCURY PLUS, Varian). It was confirmed from the obtained results that the complexes were the target compounds. Analysis Results of the Sulfonium Borate Complex of Formula (1a) [4-hydroxyphenyl-methyl-1-naphthylmethyl sulfonium tetrakis(pentafluorophenyl)borate] M+ = 281 (sulfonium residue)M+ = 679 (borate residue) Actual Measured Values: C 52.51, H 1.89Theoretical Values: C 52.52, H 1.78-1)> 662 (C-S), 776, 980, 1088, 1276 (Ar-F), 1300, 1374, 1464, 1514, 1583, 1643, 2881 (C-H), 2981 (C-H), 3107 (O-H)<1H-NMR Analysis Results (δ value), Refer to Fig. 1 (Using THF)> 2.6 (1H, (d)), 3.3 (3H, (a)), 5.3 (2H, (e)), 6.9 (2H, (c)), 7.6 (2H, (b)), 7.2-8.1 (7H, (f), (g), (h), (i), (j), (k), (1))(Proton assignment) [Show Image] Analysis Results of the Sulfonium Borate Complex of Formula (1b) [4-hydroxyphenyl-methyl-(2-methylbenzyl) sulfonium tetrakis(pentafluorophenyl)borate] M+ = 245 (sulfonium residue)M+ = 679 (borate residue) Actual Measured Values: C 50.39, H 1.77Theoretical Values: C 50.60, H 1.80-1)> 662 (C-S), 773, 980, 1088, 1276 (Ar-F), 1463, 1514, 1583, 1644, 2882 (C-H), 2983 (C-H), 3.109 (O-H)<1H-NMR Analysis Results (δ value), Refer to Fig. 2 (Using THF)> 2.3 (3H, (j)), 2.4 (1H, (d)), 3.3 (3H, (a)), 4.8 (2H, (e)), 7.0 (2H, (c)), 7.6 (2H, (b)), 7.0-7.4 (4H, (f), (g), (h), (i))(Proton assignment)
In water; ethyl acetate at 20℃; for 0.5h; 1 Sulfonium antimonate complexes of the formulas (1d), (1e) and (1f) were prepared by dissolving the sulfonium antimonate complex (see Japanese Patent Application Laid-open No. 10-245378 for the synthesis method) in ethyl acetate to prepare a 10% by mass ethyl acetate solution of the complex .Apart from these, a 10% by mass aqueous solution of the sodium borate salt synthesis formula (3) was prepared as disclosed in JP-A No. 10-310587).Next, a 10% by mass aqueous solution of the sodium borate salt of the formula (3) was mixed with equimolar amount of the room temperature ethyl acetate solution of the complex at room temperature and stirred as it was for 30 minutes. Thereafter, the ethyl acetate layer was separated from the reaction mixture, dried and ethyl acetate was removed under reduced pressure.As the evaporation residue, a sulfonium borate complex of the formula (1a) of Example 1, a sulfonium borate complex of the formula (1b) of Example 2 and a sulfonium borate complex of the (1c) of the Comparative Example 1 were obtained.
In water; ethyl acetate at 20℃; for 0.5h; 1 Sulfonium antimonate complexes of the formulas (1d), (1e) and (1f) (see JP-A 10-245378 for the synthesis method) were dissolved in ethyl acetate,A 10 mass% ethyl acetate solution of the complex was prepared. Apart from these, a 10% by mass aqueous solution of the sodium borate salt of the formula (3) (see JP-A 10-310587 for the synthesis method) was prepared.next,To a 10% by mass ethyl acetate solution of the complex, A 10 wt% aqueous solution of the sodium borate salt of the formula (3) Mixed in equimolar amount at room temperature, The mixture was stirred for 30 minutes.after that, The ethyl acetate layer was separated from the reaction mixture, Dried,Ethyl acetate was removed under reduced pressure.As evaporation residue,The sulfonium borate complex of the formula (1a) of Example 1,The sulfonium borate complex of the formula (1b) of Example 2 and Comparative Example 1 of formula (1c) sulfonium borate complex was obtained.
  • 5
  • [ 1073-72-9 ]
  • [ 133152-67-7 ]
YieldReaction ConditionsOperation in experiment
Multi-step reaction with 2 steps 1: water / 20 h / 35 °C 2: Isopropyl acetate / 1 h / 5 °C
  • 6
  • [ 86-52-2 ]
  • [ 133152-67-7 ]
YieldReaction ConditionsOperation in experiment
Multi-step reaction with 2 steps 1: water / 20 h / 35 °C 2: Isopropyl acetate / 1 h / 5 °C
  • 7
  • sodium hexafluoroantimonate [ No CAS ]
  • 4-hydroxyphenyl(α-naphthylmethyl) methylsulfonium chloride [ No CAS ]
  • [ 133152-67-7 ]
YieldReaction ConditionsOperation in experiment
93% In Isopropyl acetate at 5℃; for 1h; 3 Synthesis of 4-hydroxyphenyl (α- naphthylmethyl) methyl hexafluoroantimonate 4-hydroxy-phenyl methyl sulfide 14.5g (0.103 mol), α- naphthyl methyl chloride 18.2g (0.103mol), water 180ml allowed to react for 20 hours at 35 ° C, 4- hydroxyphenyl (α-naphthylmethyl) methyl to obtain an aqueous solution of the sulfonium chloride 32.7g (0.103mol). This isopropyl acetate 200mL was added, and then was charged with sodiumhexafluoroantimonate 26.6g (0.103 mol), and react for 1 hour at 5 ° C. After the reaction, togive a white crystals were treated in the same manner as in Example 1. Obtained product was 49.5g.NMR analysis, the results of IR analysis and elemental analysis, the product was confirmed to be notation. Yield 93.0% and a melting point of 125.0127.0 ° C. The content concentration of Naions and chlorine ions was below the detection limit 1 ppm.
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