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Preparation method of imatine

An imaamine and enzymatic technology, applied in the field of preparation of imaamine, can solve the problems of low product yield, long reaction route and high cost, and achieve the effects of high product conversion rate and low impurity content

Active Publication Date: 2021-02-12
江苏八巨药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention aims at the defects existing in the above prior art, and provides a preparation method of imamamine, in order to solve the existing problems of long reaction route, high cost and low product yield

Method used

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  • Preparation method of imatine
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  • Preparation method of imatine

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Experimental program
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Effect test

Embodiment 1

[0020] In the clean reactor, add water 100g, ethanol 20g, then add raw material N-(2-methyl-5-nitrophenyl)-4-(3-pyridyl)-2-pyrimidinamine 50g, adopt SEQ ID NO 1. Add 2 g of nitroreductase and 0.2 g of coenzyme, stir, slowly raise the temperature to 37 ° C for 2 hours of reaction, after the reaction, collect the filtrate after suction filtration, perform vacuum distillation to remove solvent ethanol, suction filtration, and dry Dry to obtain the corresponding product 44.1g imamamine, the yield is 97.8%, and the liquid phase (HPLC) detection content is 99.5%.

Embodiment 2

[0022] Add water 100g, ethanol 20g, N-(2-methyl-5-nitrophenyl)-4-(3-pyridyl)-2-pyrimidinamine 50g successively in clean reactor, adopt SEQ ID NO 1 2g of the shown nitroreductase, 0.2g of coenzyme, stirring, slowly heating up to about 35°C for reaction and heat preservation for 2h, suction filtration, distillation to remove solvent ethanol, suction filtration, drying to obtain 44.0g of the corresponding product imamamine, The yield is 97.6%, and the liquid phase (HPLC) detection content is 99.6%.

Embodiment 3

[0024] Add water 100g, methanol 20g, N-(2-methyl-5-nitrophenyl)-4-(3-pyridyl)-2-pyrimidinamine 50g successively in clean reactor, adopt SEQ ID NO 1 .The nitroreductase 2g shown, the coenzyme 0.2g, the temperature is raised to about 37 ℃, the reaction is incubated for 2h, the solvent ethanol is distilled off by suction filtration, the solvent ethanol is distilled off, the corresponding product 44.3g imamamine is obtained, and the yield is 98.2 %, liquid phase (HPLC) detection content 99.5%.

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Abstract

The invention relates to a preparation method of imatine, and belongs to the technical field of medicine synthesis. In order to solve the problem of low product yield in the prior art, the invention provides the preparation method of the imatrine, which comprises the following steps: under the action of a catalytic amount of nitroreductase and coenzyme, converting a compound N-(2-methyl-5-nitrophenyl)-4-(3-pyridyl)-2-pyrimidinamine shown as a formula II into the imatrine through an enzymatic reaction; wherein the nitroreductase is as shown in SEQ NO1. According to the method, nitryl can be effectively and efficiently converted into amino, other by-products cannot be generated due to side reaction of the raw materials in the reaction process, the method has the advantages of being low in impurity content and high in product conversion rate, and the product yield reaches 97% or above.

Description

technical field [0001] The invention relates to a preparation method of imaamine, which belongs to the technical field of drug synthesis. Background technique [0002] Imatinib mesylate is the first-generation tyrosine kinase inhibitor, which can specifically block the signal transduction of chronic myeloid leukemia, thereby blocking the proliferation of tumor cells, and is clinically used for Philadelphia chromosome-positive The treatment of chronic myelogenous leukemia, but also the treatment of patients with gastrointestinal stromal tumors. [0003] And imaamine is as the intermediate of imatinib mesylate, at present, existing mainly is N-(2-methyl-5-nitrophenyl)-4-(3-pyridyl)-2 -Pyrimidinamine obtains corresponding imamamine through palladium-carbon hydrogenation reduction, but, wherein the catalyst palladium-carbon etc. that adopt is expensive, and hydrogenation process is also more dangerous, obtains product yield and purity low, is not suitable for suitability for in...

Claims

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Application Information

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IPC IPC(8): C12P17/16
CPCC12P17/165
Inventor 程加铭付自强陈恬胡建涛王建军张锦涛
Owner 江苏八巨药业有限公司
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