Preparation method of trimethylsilyl trifluoromethanesulfonate

Abstract

The invention discloses a preparation method of trimethylsilyl trifluoromethanesulfonate, which comprises the following steps: adding anhydrous trifluoromethanesulfonic acid and anhydrous trimethylchlorosilane into a reaction vessel, and reacting at 10-30 DEG C for 12 hours while stirring under an inert gas protective atmosphere; and after the reaction is finished, performing reduced pressure distillation for 1-2 hours, and collecting the distillate of 125-135 DEG C, which is the trimethylsilyl trifluoromethanesulfonate. According to the method, no side reaction exists in the preparation process; the product is high in purity and yield and low in cost; and the purity of the product is up to 99.9%, and the yield of the product is up to 97.8%.

Description

technical field [0001] The invention relates to a preparation method of trimethylsilyl trifluoromethanesulfonate, which belongs to the field of fine chemicals. Background technique [0002] Trimethylsilyl trifluoromethanesulfonate is often used as a catalyst for silylation reagents or a cationic initiator in organic synthesis reactions. At present, there are two commonly used preparation methods, one is through trifluoromethanesulfonic acid and tetramethyl However, tetramethylsilane often contains a large amount of impurities such as dimethylbutane, dimethylchlorosilane, and methyldichlorosilane in the preparation process, and the above-mentioned impurities are easily mixed with trifluoromethanesulfonic acid Side reactions occur, especially the boiling point of trifluoromethanesulfonate dimethyl silicone grease and trimethylsilyl trifluoromethanesulfonate generated by dimethyl chlorosilane and trifluoromethanesulfonic acid is very close, so it is difficult to use rectificati...

AI Technical Summary

Problems solved by technology

[0002] Trimethylsilyl trifluoromethanesulfonate is often used as a catalyst for silylation reagents or a cationic initiator in organic synthesis reactions. At present, there are two commonly used preparation methods, one is through trifluoromethanesulfonic acid and tetramethyl However, tetramethylsilane often contains a large amount of impurities such as dimethylbutane, dimethylchlorosilane, and methyldichlorosilane in the preparation process, and the above-mentioned impurities are easily mixed with trifluoromethanesulfonic acid Side reactions occur, especially the boiling point of trifluoromethanesulfonate dimethyl silicone grease and trimethylsilyl trifluoromethanesulfonate generated by dimethyl chlorosilane and trifluoromethanesulfonic acid is very close, so it is difficult to use rectification Method separation will bring great difficulties to the purification and separation of trimethylsilyl trifluoromethanesulfonate; another preparation method is through the reaction of trifluoromethanesulfonate and silylating reagent, this preparation method Trimethylsilyl trifluoromethanesulfonate with a purity of up to 99.9% can be obtained, but this preparation method requires an excessive amount of silylation reagent, which increases the preparation cost