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Method for preparing tianeptine sodium intermediate

A technology for tianuptine sodium and intermediates, which is applied in the field of preparation of pharmaceutical intermediates, can solve the problems of large waste water, serious pollution, and high energy consumption, and achieve the effects of less three wastes, no discharge of three wastes, and high purity

Active Publication Date: 2014-09-10
山东诚汇双达药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are not many reports on its synthetic method in the literature, and the preparation method of intermediate A is mostly prepared from intermediate B raw material, which is prepared through multi-step reactions: among them, it needs to be hydrolyzed by strong alkali for a long time at high temperature or high-risk sodium hydride hydrolysis, acyl thionyl chloride Chemical, and then catalyzed by Lewis acid (such as aluminum trichloride) to obtain, in mass production, high energy consumption, serious pollution, huge amount of waste water

Method used

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  • Method for preparing tianeptine sodium intermediate
  • Method for preparing tianeptine sodium intermediate
  • Method for preparing tianeptine sodium intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Catalytic preparation of intermediate A by polyphosphoric acid

[0032] Add 339KG of intermediate B into a 2000L reactor, slowly add 700KG of polyphosphoric acid, turn on the steam and heat to about 40 degrees, turn on the stirring, raise the temperature to 75 degrees and react for 4 hours. The complete conversion of intermediate B was monitored by liquid phase, the temperature was lowered to 30°C, poured into 800KG of ice water, continued to cool down to 10°C, kept warm and crystallized for 2 hours, and centrifuged to obtain a white solid with a wet weight of 386KG, HPLC: 98.2%.

[0033] Transfer the obtained solid to the reaction kettle, which contains 1300KG of 95% ethanol in advance. After heating and dissolving completely, cool down to 5 degrees to crystallize for 4 hours, centrifuge and dry the refined product at 60 degrees to obtain a total of 292KG of finished products, with a yield of 95.1 %, HPLC: 99.8%

[0034] The refined mother liquor is distilled and conc...

Embodiment 2

[0037] Catalyzed Preparation of Intermediate A by Sulfuric Acid

[0038] Add 339KG of intermediate B into a reactor containing 780KG of concentrated sulfuric acid, raise the temperature to 40°C, start stirring, continue to heat up to 65°C, and react for 5 hours. High-efficiency liquid phase monitors the complete conversion of intermediate B, lowers the temperature to 20 degrees, and slowly transfers the reaction solution to a reactor containing 1000KG of ice water, and cools the temperature with ice-salt water, and the temperature control is not higher than 50 degrees. After the transfer is completed, cool down to 8 degrees and crystallize for 3 hours, and centrifuge to obtain a white solid with a wet weight of 389KG, HPLC: 98.8%

[0039] The obtained solid was transferred to the reaction kettle, and there was 1400KG of pre-injected methanol in the kettle. After heating and dissolving completely, the temperature was lowered to 6 degrees to crystallize for 6 hours. HPLC: 99.9%...

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Abstract

The invention discloses a method for preparing a tianeptine sodium intermediate 3-chloro-6-methyl dibenzo[c, f][1, 2] thiazepine-11-(6H)-ketone 5,5-dioxide. 4-chloro-2-(N-methyl-N-phenyl-sulfamoyl)-methyl benzoate is taken as a raw material for synthesizing the tianeptine sodium intermediate in one step. Compared with the prior art, the synthesis method is simple and convenient and has relatively good economic benefit.

Description

technical field [0001] The invention relates to the technical field of preparation of pharmaceutical intermediates, in particular to a preparation method of a tianuptine sodium intermediate. Background technique [0002] Tianeptine is an antidepressant with significantly fewer adverse effects than tricyclic antidepressants. It has the following effects on animals: increasing the spontaneous activity of cone cells in the hippocampus, accelerating the recovery after functional inhibition, and accelerating the uptake of 5-hydroxytryptamine by neurons in the cerebral cortex and hippocampus. Tianeptine has the following action characteristics on the human body: the effect on mood disorders, in the two classifications of sedative and excitatory antidepressants, the effect of this drug is between the two. It has a significant effect on somatic symptoms, especially gastrointestinal symptoms related to anxiety and mood disorders. It has a relieving effect on the abnormal personalit...

Claims

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Application Information

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IPC IPC(8): C07D281/02
CPCC07D281/02
Inventor 葛正全胡俊峰王庭见杨彦军
Owner 山东诚汇双达药业有限公司
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