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Preparation method of cinepazide maleate

A technology for the preparation of cinepazide maleate and its preparation steps, which is applied in the field of preparation of cinepazide maleate, can solve the problems of limited application, high toxicity, cumbersome handling, etc., and achieve high raw material utilization, low cost, The effect of easy process control

Inactive Publication Date: 2009-12-16
SHANGHAI INST OF PHARMA IND +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0018] CN1631877A adds excessive pyrrolidine as acid-binding agent, reacts in methylene chloride, and aftertreatment is more loaded down with trivial details
[0019] CN1876646A has adopted chloroform as solvent, and toxicity is bigger, and application is restricted

Method used

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  • Preparation method of cinepazide maleate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] Synthesis of Chloroacetylpyrrolidine (II)

[0067] Chloroacetyl chloride (135g, 1.2mol) and dichloromethane (340ml) were added to a 1-liter reaction flask, cooled to -10°C in an ice-salt bath, and triethylamine (127g, 1.26mol) and pyrrolidine (85g, 1.2mol) and dichloromethane (340ml) mixed solution, control the temperature below 5 ° C, about 2 hours to complete the addition. Stir at 0-5°C for 1 hour, and at room temperature for another 1 hour. Suction filtration, the filter cake was washed with dichloromethane (510ml), and dried to obtain a brown filtrate. After the filtrate was washed with water (150ml×3), it was concentrated to obtain 158g of a brown oily substance, with a yield of 90%.

Embodiment 2

[0069] Synthesis of 1-piperazine acetylpyrrolidine (IV)

[0070] Piperazine dihydrochloride (13.28g, 0.075mol), water 70ml, anhydrous piperazine (5.60g, 0.065mol), chloroacetylpyrrolidine (7.38g, 0.05mol), use method 1, react for 7h, and then put into Anhydrous piperazine (4.31g, 0.05mol), and 40ml aqueous solution of chloroacetylpyrrolidine (7.38g, 0.05mol) were added dropwise again, and reacted for 7h, and fed in this way until 4 batches of chloroacetylpyrrolidine were added in total. 33.6 g of 1-piperazine acetylpyrrolidine was obtained, with a melting point of 65° C. and a yield of 85.12%.

Embodiment 3

[0072] Synthesis of 1-piperazine acetylpyrrolidine (IV)

[0073] Piperazine dihydrochloride (13.28g, 0.075mol), water 60ml, piperazine hexahydrate (12.62g, 0.065mol), chloroacetylpyrrolidine (7.38g, 0.05mol), use method 2, react for 9h, and then put into Piperazine hexahydrate (9.72g, 0.05mol), and a solution formed by dissolving chloroacetylpyrrolidine (7.38g, 0.05mol) in 40ml of water was added dropwise again, reacted for 8h, and fed in a circular manner in this way until a total of 6 batches of chloroacetylpyrrole were added Pyridine, 1-piperazine acetylpyrrolidine was collected to obtain 49.88g, melting point 65°C, yield 84.28%.

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Abstract

The invention discloses a preparation method of cinepazide maleate, comprising the steps of (1) preparing 1-piperazine acetyl pyrrolidine (IV) and (2) taking 1-piperazine acetyl pyrrolidine as material to prepare cinepazide maleate. The preparation method of 1-piperazine acetyl pyrrolidine comprises the following steps: placing piperazine dihydrochloride in water to react with alkaline and obtaining a reaction system containing piperazine monohydrochloride; (2) adding chloracetyl pyrrolidine into the reaction system for reaction, adjusting pH to 10-13 by using alkaline material, collecting 1-piperazine acetyl pyrrolidine from reaction products. The method for preparing the cinepazide maleate has low cost, high material utilization ratio, simple and convenient operation and higher yield and is suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of cinepazide maleate. Background technique [0002] Cinepazide maleate (molecular formula: C 26 h 35 N 3 o 9 ), the English name is Cinepazide Maleate, and the structural formula (I) is as follows: [0003] [0004] Cinepazide maleate is a new generation of piperazine drugs, which can improve brain metabolism, inhibit the release of excitatory transmitters, promote the release of GABA, mediate ion flow channels, stabilize cell membranes, block ischemia-reperfusion injury, and fully recover Blood circulation, activation of 5-HT neurons. Clinically widely used in the treatment of cardiovascular and cerebrovascular diseases. [0005] Due to the large dosage and clinical dosage of cinepazide maleate, it is necessary to establish a process method that is easy to operate, easy to control the reaction, environmentally friendly and suitable for industrial production. [0006] At present, existing patents...

Claims

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Application Information

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IPC IPC(8): C07D295/185A61P9/00
Inventor 李建其黄雷
Owner SHANGHAI INST OF PHARMA IND
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