Preparation method of nimodipine

A nimodipine, reaction technology, applied in the field of preparation of nimodipine, can solve the problem of low process yield, achieve high yield, reduce raw material cost, and achieve good quality effects
CN102174012AActive Publication Date: 2011-09-07SHANDONG XINHUA PHARMA CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
SHANDONG XINHUA PHARMA CO LTD
Publication Date
2011-09-07

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Abstract

The invention belongs to the technical field of pharmacy, and in particular relates to a preparation method of nimodipine, comprising urethane reaction and cyclization reaction, wherein in the urethane reaction, after ammonia introducing reaction, adding an inorganic salt for dewatering the urethane reaction liquid, then rectifying to obtain isopropyl-3-aminocrotonate; and performing cyclization reaction with 2-(3-nitrobenzylidene)-acetoacetic acid-2-methoxyethyl ester by taking fatty alcohol as a reaction solvent. The invention has the advantages of high product yield and good quality, the primary yield can reach 85-89%, the solvent can be recovered for use, the raw material cost can be greatly reduced, and the content of total impurities is decreased from 0.4-1.0% of the original process to 0.1-0.3% by HPLC (High Performance Liquid Chromatography) detection.
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Description

technical field

[0001] The invention belongs to the technical field of pharmacy, and in particular relates to a preparation method of nimodipine. Background technique

[0002] The chemical name of Nimodipine is 2,6-dimethyl-4-(3-nitrophenyl)-1,4-dihydro-3,5-pyridinedicarboxylic acid-2-methoxyethyl -(1-methylethyl) ester, a calcium channel antagonist belonging to the dihydropyridine class, is suitable for improving blood circulation in cerebral vasospasm after subarachnoid hemorrhage of various causes and in the recovery period of acute cerebrovascular disease. The synthetic technique of nimodipine adopts the following steps at present:

[0003] A. Urethane reaction:

[0004]

[0005] B. Cycling reaction

[0006]

[0007]

[0008] Because the urethane reaction generates water in the process of passing through the ammonia, the reaction liquid after the completion of passing through the ammonia in the original process is directly rectified. Due to the existence of w...

Claims

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