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A kind of aftertreatment method of moclobemide intermediate

A moclobemide and intermediate technology, applied in the field of moclobemide intermediate post-processing, can solve the problems of large environmental pollution and high solvent loss, and achieve the effects of significant environmental protection, improved purity and reduced consumption

Active Publication Date: 2016-02-03
JIANGSU RUIKE MEDICAL SCI & TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Moclobemide intermediates are generally crystallized in toluene solution in the existing process, and the toluene gas volatilized during the centrifugation process has great environmental pollution and high solvent loss

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Using ethisulfate and p-chlorobenzoyl chloride as raw materials, triethylamine as an acid-binding agent, and toluene as a solvent, synthesize the key intermediate p-chlorobenzamide ethylsulfate of moclobemide at 0°C, and react After the end, add 8 times the amount of water of the mixed solution after the reaction, and raise the reaction solution to 30-35 ° C to dry, so that all the solids generated are dissolved, and the layers are left to stand, and the separated organic layer toluene is separated by distillation with water. Remove the water, and use the recovered toluene; the water layer is cooled to 15°C, crystallized for half an hour, centrifuged to dryness, washed with 1 times the amount of water, centrifuged to dryness, and dried to dryness in a vacuum of -0.080MPa and 25°C. Crushing and bagging, the yield is 92.75%, and the content is 90.52%.

Embodiment 2

[0017] Using ethisulfate and p-chlorobenzoyl chloride as raw materials, triethylamine as an acid-binding agent, and toluene as a solvent, synthesize the key intermediate p-chlorobenzamide ethylsulfate of moclobemide at 5°C, and react After the end, add 10 times the amount of water of the mixed solution after the reaction, and raise the reaction solution to 30-35 ° C for drying, so that all the solids generated are dissolved, and the separated organic layer toluene is separated by distilling with water. Remove the water, and use the recovered toluene; the water layer is cooled to 20°C, crystallized for half an hour, centrifuged to dryness, washed with 2 times the amount of water, centrifuged to dryness, and dried to dryness at -0.100MPa in vacuum at 30°C. Crushing and bagging, the yield is 91.68%, and the content is 91.82%.

[0018] It is not difficult to see that the present invention is to add 8 to 10 times the amount of water after the reaction of the key intermediate p-chlo...

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PUM

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Abstract

A disclosed post-processing method for a moclobemide intermediate comprises: taking ethylammonium sulfate and 4-chlorobenzoyl chloride as raw materials, taking triethylamine as an acid-binding agent, and taking toluene as a solvent, synthesizing the moclobemide key intermediate 4-chlorobenzamidoethyl sulfate at 0-5 DEG C; after the reaction is finished, adding water being 8-10 times of the reaction mixed solution, AND heating the mixed solution to 30-35 DEG C, so as to completely dissolve generated solid, standing for layering; distilling to separating water in the organic layer toluene and recycling toluene; AND cooling the water layer to 15-20 DEG C for half an hour, centrifuging to dry, then using water being 1-2 times to wash, centrifuging to dry, and drying under the vacuum condition of 0.080-0.100 MPa at 25-30 DEG C. The method realizes efficient recovery of toluene, also improves the product quality, and has substantial environment-protection benefit and economic benefit.

Description

technical field [0001] The invention belongs to the field of medicine and chemical industry, in particular to a post-treatment method of a moclobemide intermediate. Background technique [0002] Moclobemide intermediates are generally crystallized in toluene solution in the existing process, and the toluene gas volatilized during the centrifugation process has great environmental pollution and high solvent loss. The final product has many impurities and low content. Contents of the invention [0003] The purpose of this section is to outline some aspects of embodiments of the invention and briefly describe some preferred embodiments. Some simplifications or omissions may be made in this section, as well as in the abstract and titles of this application, to avoid obscuring the purpose of this section, the abstract and titles, and such simplifications or omissions should not be used to limit the scope of the invention. [0004] In view of the above and / or the problems exis...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C305/04C07C303/44
Inventor 赵小泉陆华朱家伍何蒲军匡立幸
Owner JIANGSU RUIKE MEDICAL SCI & TECH CO LTD