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

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0021] The embodiment of the present invention provides a method for synthesizing trimethylsilyl acetate, which includes the following steps: adding 0.63 to 0.84 parts of sodium acetate, 0.5 to 5 parts of solvent, and 0.0001 to 0.005 parts of phase transfer catalyst into a reaction kettle in parts by mass. Stir uniformly at a temperature of 20℃~30℃, add 1 part of trimethylchlorosilane dropwise to the reactor under the condition of a dropping rate of 1g / min~2g / min, and stir at a temperature of 10℃~60℃ React for 2h~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 pressure of one atmosphere to collect the distillate at 106℃~108℃ to obtain trimethylsilyl acetate. Fat products.

[0022] GC (Gas Chromatography) was used to detect the trimethyl silicone acetate product, and the content of trimethyl silicone acetate in the trimethyl silicone acetate product was 98% to 98.5%.

[0023] From th...

Example Embodiment

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

[0027] In a 1000ml four-neck glass round-bottom flask, add 86g sodium acetate, 209g N,N-dimethylformamide and 0.216g tetrabutylammonium chloride. The four-neck glass round-bottom flask is equipped with a stirrer, a thermometer, and reflux condensation. Tube, constant pressure funnel and heater. At a temperature of 30°C, stir the sodium acetate, N,N-dimethylformamide and tetrabutylammonium chloride uniformly, add 108.5g of trimethylchlorosilane to the constant pressure funnel, and remove the drops of the constant pressure funnel. The acceleration was adjusted to 2g / min; the trimethylchlorosilane in the constant pressure funnel was dropped into a four-neck glass round bottom flask. After the dropwise addition of trimethylchlorosilane is completed, the temperature is raised to 60°C and the reaction is stirred for 2h to obtain the liquid to be filtered. ...

Example Embodiment

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

[0029] In a 1000ml four-neck glass round-bottom flask, add 98.4g sodium acetate, 542.5g N,N-dimethylacetamide and 0.54g tetrabutylammonium bromide. The four-neck glass round-bottom flask is equipped with a stirrer, thermometer and reflux. Condensation tube, constant pressure funnel and heater. At a temperature of 20°C, stir the sodium acetate, N,N-dimethylacetamide and tetrabutylammonium bromide uniformly, add 108.5g of trimethylchlorosilane to the constant pressure funnel, and remove the drops of the constant pressure funnel. The acceleration is adjusted to 1g / min, and the trimethylchlorosilane in the constant pressure funnel is dropped into a four-neck glass round bottom flask. After the trimethylchlorosilane is added, the temperature is raised to 40°C, and the reaction is stirred for 3h to obtain the filter Liquid, the filtrate is separated from th...

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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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