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Glimepiride intermediate preparation method

An intermediate and ethyl technology, applied in the field of medicine, can solve the problems of long reaction time, highly toxic NaCN material, human and environmental hazards, etc., and achieve the effects of improving market competitiveness, reducing production costs, and reducing contact opportunities.

Inactive Publication Date: 2017-05-17
山东康倍得生物医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Among them, cyanidation and extraction and refining are the bottleneck links. The traditional cyanidation process uses sodium bisulfite and solid sodium cyanide as raw materials of NaCN (solid) / NaHSO 3 ) (solid) cyanide system, the solid material needs to be transported and dissolved manually, and the NaCN material is highly toxic, labor-intensive, the reaction process material is sticky and sticky, difficult to stir, the reaction time is long, the yield is low, and a large amount of The waste acid of cyanide ion is not easy to handle; the product extraction and refining has always been extracted with organic solvent benzene. Above, troublesome post-processing
And benzene is a strong carcinogen, causing great harm to the human body and the environment

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0044] A kind of preparation method of glimepiride intermediate, such as figure 2 shown, including the following steps:

[0045] (1) Using ethyl acetoacetate as a raw material, in the presence of a strong base, sodium ethoxide, through bromoethane substitution reaction, to generate ethyl 2-ethyl-3-oxobutanoate;

[0046] (2) 2-ethyl-3-oxobutanoic acid ethyl ester generates 2-ethyl-3-hydroxyl-3-cyanobutanoic acid ethyl ester through reaction with NaCN / sulfuric acid cyanation system in the cyanidation reactor, Such as figure 1 Shown, the special equipment that uses comprises cyanide reactor 1 and pickling tank 2, and the top of described cyanide reactor 1 is connected with NaCN metering tank 3 and sulfuric acid dropping tank 4; The top of described pickling tank 2 is connected There is an acid washing metering tank 5; and the bottom of the cyanidation reaction kettle 1 is connected to the top of the pickling kettle 2 by a pipeline, and the bottom of the pickling kettle 2 is co...

Embodiment 2

[0059] A preparation method of glimepiride intermediate, comprising the steps of:

[0060] (1) Using ethyl acetoacetate as a raw material, in the presence of a strong base, sodium ethoxide, through bromoethane substitution reaction, to generate ethyl 2-ethyl-3-oxobutanoate;

[0061] (2) 2-ethyl-3-oxobutanoic acid ethyl ester generates 2-ethyl-3-hydroxyl-3-cyanobutanoic acid ethyl ester through reaction with NaCN / sulfuric acid cyanation system in the cyanidation reactor, The special equipment that uses comprises cyanide reactor and pickling tank, and the top of described cyanide reactor is connected with NaCN metering tank and sulfuric acid dropping tank; The top of described pickling still is connected with washing acid metering tank; The lower part of the cyanide reaction kettle is connected to the top of the pickling kettle by a pipeline, and the bottom of the pickling kettle is connected back to the sulfuric acid dropping tank by a pipeline;

[0062] The detailed process i...

Embodiment 3

[0074] A preparation method of glimepiride intermediate, comprising the steps of:

[0075] (1) Using ethyl acetoacetate as a raw material, in the presence of a strong base, sodium ethoxide, through bromoethane substitution reaction, to generate ethyl 2-ethyl-3-oxobutanoate;

[0076] (2) 2-ethyl-3-oxobutanoic acid ethyl ester generates 2-ethyl-3-hydroxyl-3-cyanobutanoic acid ethyl ester through reaction with NaCN / sulfuric acid cyanation system in the cyanidation reactor, The special equipment that uses comprises cyanide reactor and pickling tank, and the top of described cyanide reactor is connected with NaCN metering tank and sulfuric acid dropping tank; The top of described pickling still is connected with washing acid metering tank; The lower part of the cyanide reaction kettle is connected to the top of the pickling kettle by a pipeline, and the bottom of the pickling kettle is connected back to the sulfuric acid dropping tank by a pipeline;

[0077] The detailed process i...

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Abstract

The invention relates to a glimepiride intermediate preparation method which comprises the following steps: 1, using ethyl acetoacetate as a raw material and generating 2-ethyl-3-oxobutanoate through bromoethane substitution reaction in the presence of strong-base sodium ethoxide; 2, generating 2-ethyl-3-hydroxy-3-cyanoethyl butyrate through NaCN / sulfuric acid cyaniding system reaction in a cyaniding reaction kettle; 3, cyclization generating 3-ethyl-4-methyl-1-acetyl-3-pyrroline-2-one through high-pressure catalytic hydrogenation; 4, alkali hydrolyzing to generate 3-ethyl-4-methyl-3-pyrroline-2-one through sodium carbonate solution; 5, extracting 3-ethyl-4-methyl-3-pyrroline-2-one through ethyl acetate and recrystallizing and refining to obtain a product. The method can improve product yield, also improves technological operation convenience and reduces pollution.

Description

technical field [0001] The invention relates to the technical field of medicine, in particular to a preparation method of glimepiride intermediate 3-ethyl-4-methyl-3-pyrrolin-2-one. Background technique [0002] Glimepiride is an important drug for the treatment of type II diabetes, and 3-ethyl-4-methyl-3-pyrroline-2-one is its important key intermediate. , cyanidation, reductive cyclization, hydrolysis, extraction and refining five steps to synthesize the product. [0003] Among them, cyanidation and extraction and refining are the bottleneck links. The traditional cyanidation process uses sodium bisulfite and solid sodium cyanide as raw materials of NaCN (solid) / NaHSO 3 ) (solid) cyanide system, the solid material needs to be transported and dissolved manually, and the NaCN material is highly toxic, labor-intensive, the reaction process material is sticky and sticky, difficult to stir, the reaction time is long, the yield is low, and a large amount of The waste acid of c...

Claims

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Application Information

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IPC IPC(8): C07D207/38
CPCC07D207/38
Inventor 孙新占于洪波
Owner 山东康倍得生物医药科技有限公司
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