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Method for synthesis of high purity di(trimethyl silicon based) ethanamide

A technology of trimethylsilyl and trimethylsilyl imidazole, which is applied in the field of synthesizing high-purity bisacetamide, can solve the problems of low reaction yield, large environmental pollution, easy decomposition of products, etc., and achieves high purity and simplified process. Process, the effect of reducing the production of by-products acetonitrile and silyl ethers

Inactive Publication Date: 2011-05-25
ZHEJIANG UNIV +1
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Problems solved by technology

Therefore, in various methods for synthesizing BSA, there are generally problems such as low reaction yield, poor selectivity, easy decomposition of products, and large environmental pollution.

Method used

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  • Method for synthesis of high purity di(trimethyl silicon based) ethanamide
  • Method for synthesis of high purity di(trimethyl silicon based) ethanamide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Add 33.6g (0.24mol) trimethylsilyl imidazole and 1.5g (0.01mol) 2-mercaptobenzo Thiazole, and a mixture of 12g (0.2mol) acetamide and 33.6g (0.24mol) trimethylsilyl imidazole was added to a constant pressure dropping funnel. Then heat, turn on magnetic stirring, depressurize, control the reaction pressure to a vacuum of 0.08MPa, control the temperature of the reactor at about 160°C, slowly add the mixed solution dropwise from the constant pressure funnel, rectify while reacting, and collect the The fraction is the crude BSA product, and the reaction time is controlled to be 5 hours. Then, the BSA crude product is rectified to obtain a high-content pure BSA product with a yield of 85% and a content of 99.2%.

Embodiment 3-8

[0019] Similar to Example 1, the control reaction pressure is a vacuum of 0.08MPa, the reaction temperature is 160° C., the reaction time is 5 hours, and the type of catalyst and the amount of catalyst are changed. The reaction results are as follows (Table 1):

[0020] Table 1 Effects of different catalyst types and amounts on the reaction

[0021]

Embodiment 9-14

[0023] Similar to Example 1, using 2-mercaptobenzimidazole as a catalyst, the molar ratio of 2-mercaptobenzimidazole and acetamide is 0.001: 1, and the molar ratio of trimethylsilimidazole and acetamide is 2.4: 1, changing The condition of temperature of reaction, reaction pressure and reaction time, reaction result is as following table (table two):

[0024] Table 2 The influence of different reaction conditions on the reaction

[0025]

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Abstract

The present invention relates to a method for synthesizing high-purity di-(trimethylsilyl)acetamide, which uses N-trimethylsilylimidazole and acetamide as materials and mercapto-compound as catalyst and adopts the reactive distillation technology to synthesize the high-purity di-(trimethylsilyl)acetamide. The molar ratio of the N-trimethylsilylimidazole and the acetamide is 5:1 to 1:5; the molar ratio of the catalyst and the acetamide is 1:10000 to 1:100; and under conditions that vacuum degree is 0.01MPa to 0.09Mpa and the temperature is 100 DEG C to 200 DEG C, the reaction lasts for one to twenty hours until the high-purity di-(trimethylsilyl)acetamide is prepared. The method has the advantages of high reaction yield, little by-product, high product purity, little pollution, and the like.

Description

technical field [0001] The invention relates to a method for synthesizing high-purity bis(trimethylsilyl)acetamide by reactive distillation technology using trimethylsilimidazole and acetamide as raw materials in the presence of a catalyst. Background technique [0002] Bis(trimethylsilyl)acetamide, referred to as BSA, is an important pharmaceutical intermediate, which is mainly used as a neutral silylating agent in the silylation protection of amino acids, carboxylic acids, alcohols and amides, especially in cephalosporins Widely used in the synthesis of antibiotics. Cephalosporin antibiotics are a class of antibiotics with the fastest development, the most varieties and the fastest speed in foreign countries since the 1970s. Because of its wide antibacterial spectrum, strong bactericidal power, high stability to β-lactamase, lower toxic and side effects than semi-synthetic penicillins, and good clinical efficacy, it still ranks first among all kinds of antibiotics in the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/08B01J31/02
CPCY02P20/10
Inventor 王从敏胡文江吴建平陈思先
Owner ZHEJIANG UNIV
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