Isobutyramide preparation method

A technology of isobutyramide and isobutyronitrile, applied in the field of preparation of isobutyramide, can solve the problems of complex process, low yield, difficult environmental protection requirements, etc., and achieve the effects of simple preparation process, mild reaction conditions, and easy industrialization

Active Publication Date: 2016-07-27
XIANGSHUI MODERN CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the product purity of the isobutyramide obtained by this method for preparing isobutyramide has reached 99.87%, this method has the following disadvantages: the first is because the isobutyryl chloride used is very easy to react with water, in order to avoid Isobutyryl chloride decomposes in contact with water and other substances, and the solvent and other raw materials need to be strictly dewatered, and the reaction equipment needs to be strictly sealed. The reaction process of isobutyryl chloride and ammonia is extremely violent, so the control of the reaction conditions is also very demanding. Strict, these increase the difficulty of preparing isobutyramide
These result in more treatment of the three wastes, it is difficult to meet the requirements of environmental protection, and the cost of production is increased.
The 3rd is that this method process is complicated, and the yield of product is low, has only about 88%, and has used benzene organic solvent in the preparation process, makes the probability increase that contains harmful substance in the product, is exactly the extremely trace amount of organic solvent in different The presence of butanamide also has a great adverse effect on the application of the product in the medical field

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] The preparation of embodiment 1 isobutyramide

[0018] (1): The treatment of nitrile hydratase catalyst: after the fermented liquid obtained by fermentation of the nitrile hydratase production strain is separated with a 1.5mm sintered metal filter, it is washed twice with deionized water;

[0019] (2): Preparation of isobutyramide by hydration of isobutyronitrile: adding the cleaned nitrile hydratase catalyst to deionized water, the mass ratio of the amount of nitrile hydratase catalyst added to the amount of deionized water added is 0.02:1, isobutyramide The mass ratio of the amount of nitrile added to the amount of deionized water added is 0.5:1;

[0020] The corresponding amount of isobutyronitrile should be added continuously, the amount added should be gradually reduced, and the time of addition should be controlled within 2 hours. During the reaction, the temperature of the reaction system should be controlled at 20°C. React for 1 hour;

[0021] (3): Inactivatio...

Embodiment 2

[0024] Example 2 (S)-2-[(1-benzylsulfonyl)pyrrolidine-3-amino]-1-[4-(2,4,6-trimethylbenzyl)piperazine]ethanone in Use in the preparation of the intermediate for killing Nocardia stellatus ATCC19247

[0025] Antibacterial test

[0026] The antibacterial test was carried out using the classic filter paper method in this field, wherein Nocardia asteroides ATCC19247 was purchased from Shanghai Duma Biotechnology Co., Ltd.

[0027] culture medium

[0028] Nutrient agar and nutrient broth were purchased from Beijing Zhongke Chenyu Experimental Equipment Co., Ltd.

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Abstract

The invention relates to an isobutyramide preparation method.According to the method, isobutyronitrile and deionized water serve as raw materials, and under the action of a nitrile hydratase catalyst, isobutyronitrile and deionized water have a hydration reaction to generate isobutyramide, and a high-purity isobutyramide crystal product can be obtained by easily processing an isobutyramide aqueous solution.According to the method, the high-purity isobutyramide crystal product can be obtained by easily processing the isobutyramide aqueous solution, the purity of the product is as high as 99.95% or above, and the product does not contain organic solvents and other harmful components and is particularly suitable for application in the medical field.According to the method, reaction conditions are mild, operation is easy, the product yield is as high as 99% or above, the preparation process is simple, and industrialization is easy.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular, the invention relates to a preparation method of isobutyramide. Background technique [0002] Isobutyramide can selectively induce human g-globin gene transcription, coupled with the non-toxicity of isobutyramide and the longer half-life in plasma, it makes isobutyramide ideal in the treatment of b-thalassemia and sickle cell anemia Effect. Isobutyramide is also an important intermediate in the synthesis of ritonavir, a drug for the treatment of AIDS. Isobutyramide is widely used in the field of medicine, and the research on various intermediates used in its preparation process and isobutyramide is becoming a hot spot in this field. [0003] There have been some reports on the production and preparation methods of isobutyramide, mainly based on the method of reacting isobutyryl chloride and ammonia. The representative method is the preparation method of isobutyramide proposed by ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C12P13/02A01N43/60A01P1/00
CPCA01N43/60C12P13/02
Inventor 沈源张瀚文朱文明
Owner XIANGSHUI MODERN CHEM CO LTD
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