Device for purifying trimethylsilyl trifluoromethanesulfonate

Abstract

The invention discloses a device for purifying trimethylsilyl trifluoromethanesulfonate. The device comprises a box body, wherein the box body is internally provided with a distillation cavity; the left side of the box body is provided with a mounting block; the mounting block is internally provided with a drying cavity; the right end of the box body is provided with a collection box; the collection box is internally provided with a collection cavity; the left side space of the collection cavity communicates with the right side space of the distillation cavity through a short pipe; a fan and a temperature displayer are installed on the right side of the box body; the temperature displayer is located below the collection box; the fan is located above the collection box; a pump body is installed on the left side of the box body; the liquid inlet end of the pump body communicates with a connecting pipe; and the lower end of the box body is fixedly connected with a plurality of supporting columns. The device is used for dehydrating trimethylsilyl trifluoromethanesulfonate before purification, so the trimethylsilyl trifluoromethanesulfonate is prevented from being hydrolyzed; and meanwhile, temperature during distillation is detected by utilizing the temperature display, and a crude trimethylsilyl trifluoromethanesulfonate product is stirred, so purification efficiency is improved.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a device for purifying trimethylsilyl trifluoromethanesulfonate. Background technique [0002] Trimethylsilyl trifluoromethanesulfonate, the appearance is a colorless transparent liquid, easily hydrolyzed and fumes in the air, with a pungent smell, trimethylsilyl trifluoromethanesulfonate is often used as hydroxyl, carboxyl, carbonyl Such as functional group conversion and protection, and participate in the reaction of carbon-carbon bond growth carbon chain, can be used for Lewis acid catalyst and as a cationic initiator, is an important pharmaceutical intermediate and organic synthesis structural unit, but the existing trifluoromethanesulfonate There are still following problems in the preparation process of acid trimethylsilyl ester: [0003] The prior art usually adopts trifluoromethanesulfonic acid to react with tetramethylsilane or trimethylchlorosilane to prepare th...

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Problems solved by technology

[0003] The prior art usually adopts trifluoromethanesulfonic acid to react with tetramethylsilane or trimethylchlorosilane to prepare the crude product of trimethylsilyl trifluoromethanesulfonate. During the reaction, water, trifluoromethanesulfonate and acid, trimethylchlorosilane, trimethylsilanol, hexamethyldisiloxane and other materials, among which trifluoromethanesulfonic acid is easy to corrode equipment and pollute the environment, and when the impurities contain water, it will make trifluoromethanesulfonic acid Trimethylsilyl acid is easily hydrolyzed to form trifluoromethanesulfonic acid and trimethylsilanol, which will greatly increase the content of impurities in the later processing. Therefore, how to solve these problems reasonably is what we need to consider

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