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Method for producing high-purity isobutyramide

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

Inactive Publication Date: 2011-10-12
JIANGSU UNIV
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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 third is that the process of this method is complicated, the yield of the product is low, only about 88%, and benzene organic solvents are used in the preparation process, which increases the probability of containing harmful substances in the product. 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

[0016] The nitrile hydratase catalyst used was Rhodococcus Rhodococcus sp. The production strain is obtained through fermentation and cultivation, and the activity of the nitrile hydratase catalyst is 721×10 4 mg·h -1 ·ml -1 .

[0017] 20Kg of fermented liquid is filtered and separated with a 0.1mm sintered metal filter, and then washed twice with 20Kg of deionized water to remove impurities in the nitrile hydratase catalyst to obtain 1Kg of nitrile hydratase catalyst.

[0018] In order to ensure that the final concentration of isobutyramide in the reaction solution is above 30%, and the reaction time is within 4 hours, add 120Kg of deionized water to the reactor, and add 1Kg of pre-cleaned nitrile hydratase catalyst to the reaction In the reactor, the stirrer was started, and the temperature of the reactor was controlled at 25°C. Then start to add isobutyronitrile in the reactor, and flow rate reduces gradually, and the flow rate at the beginning is 18Kg / h, and the flow r...

Embodiment 2

[0023] The nitrile hydratase catalyst used was obtained from the production strain of Nocardia sp through fermentation, and the activity of the nitrile hydratase catalyst was 789×10 4 mg·h -1 ·ml -1 .

[0024] 20Kg of fermented liquid is filtered and separated with a 0.1mm sintered metal filter, and then washed twice with 20Kg of deionized water to remove impurities in the nitrile hydratase catalyst to obtain 1Kg of nitrile hydratase catalyst.

[0025] Add 120 Kg of deionized water into the reactor, add 1 Kg of nitrile hydratase catalyst cleaned in advance into the reactor, start the stirrer, and control the temperature of the reactor at 25° C. Then start to add isobutyronitrile in the reactor, and flow rate reduces gradually, and the flow rate at the beginning is 18Kg / h, and the flow rate after 1 hour is reduced to 17Kg / h, and the flow rate after 2 hours is reduced to 14Kg / h, and after 3 hours The flow rate is reduced to 10Kg / h, and a total of 54Kg of isobutyronitrile has ...

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PUM

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Abstract

The invention discloses a method for producing high-purity isobutyramide, and belongs to the field of biological engineering. Isobutyronitrile and deionized water are used as raw materials in the method; under the action of a nitrile hydratase catalyst, the isobutyronitrile and the deionized water undergo hydration reaction to generate isobutyramide; and a high-purity isobutyramide crystal product can be obtained by simply treating the obtained aqueous solution of isobutyramide. The high-purity isobutyramide crystal product can be obtained by simply treating the obtained aqueous solution of isobutyramide, the purity of the product reaches over 99.95 percent, and the product does not contain harmful components such as organic solvent and the like and is particularly applied in the field of medical treatment. The method is mild in reaction conditions and simple in operation; the yield of the product reaches over 99 percent; and the method overcomes the defect of a technology for preparing the isobutyramide by using the reaction of isobutyrylchloride and ammonia, and is simple in preparation process and easy for industrialization.

Description

technical field [0001] The invention relates to the field of bioengineering, in particular to a production method of high-purity 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. The wide application of isobutyramide in the field of medicine makes the requirement for the purity of isobutyramide very high. [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 Janitschke Lothar et al. in US Patent No. 35528814A. This method propos...

Claims

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Application Information

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IPC IPC(8): C12P13/02C07C233/05C07C231/24
CPCY02P20/584
Inventor 吴其飞王春梅黄达明崔凤杰马海乐管国强林琳孙文敬张志才
Owner JIANGSU UNIV
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