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Synthesis method of trimethylsilyl acetate

A technology of trimethylsilyl acetate and synthesis method, which is applied in chemical instruments and methods, compounds of group 4/14 elements of the periodic table, organic chemistry, etc., and can solve difficult reactions, low reactivity, and low product yields and other problems, to achieve the effect of thorough reaction and high activity

Inactive Publication Date: 2014-04-30
湖北新蓝天新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Existing trimethylsilyl acetate is prepared by the reaction of chlorosilane and acetic acid, because the reaction of chlorosilane and acetic acid is a substitution reaction, the reactivity is low, the reaction is difficult to carry out thoroughly, and the yield of the product obtained is low; The boiling point of trimethylsilyl is closer to the boiling point of the reaction by-product acetyl chloride, so the reaction product is not only difficult to separate, but also the purity of the obtained trimethylsilyl acetate is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0021] The embodiment of the present invention provides a method for synthesizing trimethylsilyl acetate, comprising the following steps: adding 0.63-0.84 parts of sodium acetate, 0.5-5 parts of solvent and 0.0001-0.005 parts of phase transfer catalyst into the reaction kettle in parts by mass, Stir evenly at a temperature of 20°C to 30°C, add 1 part of trimethylchlorosilane dropwise to the reaction kettle at a rate of 1g / min to 2g / min, and stir at a temperature of 10°C to 60°C React for 2h to 4h to obtain the liquid to be filtered, separate the filtrate from the liquid to be filtered to obtain the filtrate, distill the filtrate under the condition of one atmospheric pressure, collect the distillate at 106°C to 108°C, and obtain trimethylsilyl acetate fat products.

[0022] The trimethylsilyl acetate product is detected by GC (Gas Chromatography), and the content of trimethylsilyl acetate in the trimethylsilane acetate product is 98% to 98.5%.

[0023] By the reaction equatio...

Embodiment 1

[0026] Example 1: The selected solvent is N,N-dimethylformamide, and the phase transfer catalyst is tetrabutylammonium chloride.

[0027] In a 1000ml four-necked glass round-bottom flask, add 86g of sodium acetate, 209g of N,N-dimethylformamide and 0.216g of tetrabutylammonium chloride. Tube, constant pressure funnel and heater. At a temperature of 30°C, stir sodium acetate, N,N-dimethylformamide and tetrabutylammonium chloride evenly, add 108.5g trimethylchlorosilane to the constant pressure funnel, and drop the constant pressure funnel The acceleration was adjusted to 2 g / min; the trimethylchlorosilane in the constant pressure funnel was added dropwise to a four-necked glass round bottom flask. After the addition of trimethylchlorosilane is completed, the temperature is raised to 60°C and stirred for 2 hours to obtain the liquid to be filtered, and the liquid to be filtered is separated from the filtrate to obtain the filtrate. The filtrate is distilled under the condition ...

Embodiment 2

[0028] Example 2: The selected solvent is N,N-dimethylacetamide, and the phase transfer catalyst is tetrabutylammonium bromide.

[0029] In a 1000ml four-necked glass round-bottom flask, add 98.4g of sodium acetate, 542.5g of N,N-dimethylacetamide and 0.54g of tetrabutylammonium bromide. Condenser, constant pressure funnel and heater. At a temperature of 20°C, stir sodium acetate, N,N-dimethylacetamide, and tetrabutylammonium bromide evenly, add 108.5 g of trimethylchlorosilane to the constant pressure funnel, and drop the The acceleration was adjusted to 1g / min, and the trimethylchlorosilane in the constant pressure funnel was added dropwise to a four-necked glass round bottom flask. After the trimethylchlorosilane was added dropwise, the temperature was raised to 40°C, and the reaction was stirred for 3 hours to obtain Liquid, the liquid to be filtered is separated from the filtrate to obtain the filtrate, the filtrate is distilled under the condition of 1 atmospheric press...

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PUM

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Abstract

The invention discloses a synthesis method of trimethylsilyl acetate, and relates to a silylating reagent. The synthesis method comprises the steps of adding 0.63-0.84 part by mass of sodium acetate, 0.5-5 parts by mass of a solvent and 0.0001-0.005 part by mass of a phase transfer catalyst to a reaction kettle, and uniformly stirring at 20-30 DEG C; dropwise adding 1 part of trimethyl chlorosilane to the reaction kettle at an addition speed of 1-2g / min, stirring and reacting for 2-4 hours at 10-60 DEG C to obtain liquid to be filtered; separating the liquid to be filtered to obtain filtrate; and distilling the filtrate, collecting distillate at 106-108 DEG C to obtain a finished trimethylsilyl acetate product. The synthesis method disclosed by the invention is relatively high in reaction activity, thorough in reaction, high in yield of the finished trimethylsilyl acetate product and short in reaction time; and the finished trimethylsilyl acetate product is easy to separate, and is relatively high in purity.

Description

technical field [0001] The invention relates to a silylating agent, in particular to a method for synthesizing trimethylsilyl acetate. Background technique [0002] Trimethylsilyl acetate is a widely used trimethylsilylating reagent, mainly used for the silanization of alcohols, mercaptans, phenols, ketones, sulfonic acid, phenylacetylene, etc., and the reaction with boric acid to obtain three (three) methylsilane) borate. [0003] Existing trimethylsilyl acetate is prepared by the reaction of chlorosilane and acetic acid, because the reaction of chlorosilane and acetic acid is a substitution reaction, the reactivity is low, the reaction is difficult to carry out thoroughly, and the yield of the product obtained is low; The boiling point of trimethylsilyl is closer to the boiling point of the reaction by-product acetyl chloride, so the reaction product is not only difficult to separate, but also the purity of the trimethylsilyl acetate obtained is lower. Contents of the i...

Claims

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Application Information

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IPC IPC(8): C07F7/18
Inventor 赵家旭王治威申永张珩陈隽余波高建秋
Owner 湖北新蓝天新材料股份有限公司
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