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Enamine salt recrystallization purification method

A purification method and an enamine salt technology are applied in the field of enamine salt recrystallization and purification, can solve problems such as limited application, and achieve the effects of low cost, simple operation and high feasibility

Active Publication Date: 2020-09-08
内蒙古益泽制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, sodium salt is generally used as raw material to prepare enamine salt by chlorine chlorination, but the purity of enamine salt prepared by this method is generally 90-98%, and its impurity content is 2-10%, which seriously limits its application.
[0003] There are few reports about the purification of enamine salts at present, therefore, it is necessary to find a simple, effective and cheap enamine salt purification method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Embodiment 1: a kind of enamine salt recrystallization purification method, it comprises the following steps: be that the methanol solvent that the content is 90% purity is 92% enamine salt crude product and mass concentration is 80% by solid-liquid mass ratio is 1: 3 Mix, heat to 70°C to dissolve the crude enamine salt, cool to 10°C, stir and crystallize for 1.2 hours, filter and dry to obtain the finished enamine salt; the purity of the finished enamine salt is 99.4%, and the yield is 86%.

Embodiment 2

[0017] Embodiment 2: a kind of enamine salt recrystallization purification method, it comprises the following steps: the methanol solvent that the content is 89% purity is 93% enamine salt crude product and mass concentration is 85% by solid-liquid mass ratio is 1: 4 Mix, heat to 60°C to dissolve all the crude enamine salt, cool to 8°C, stir and crystallize for 1 hour, filter and dry to obtain the finished enamine salt; the purity of the finished enamine salt is 97%, and the yield is 90%.

Embodiment 3

[0018] Embodiment 3: a kind of enamine salt recrystallization purification method, it comprises the following steps: the methanol solvent that the mass concentration is 80% of the enamine salt crude product that content is 90% purity is 92.97% is 1 by solid-liquid mass ratio: 5 Mix, heat to 73°C to dissolve all the crude enamine salt, cool to 10°C, stir and crystallize for 1.5 hours, filter and dry to obtain the finished enamine salt; the purity of the finished enamine salt is 99.3%, and the yield is 74%.

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PUM

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Abstract

The invention discloses an enamine salt recrystallization purification method, which comprises the following steps: mixing an enamine salt crude product with a methanol solvent according to a solid-liquid mass ratio of 1:(1-5), heating until the solid is completely dissolved, cooling to 5-30 DEG C, crystallizing, filtering, and drying to obtain an enamine salt finished product. According to the method, by selecting the recrystallization solvent and controlling the parameters such as the dosage of the recrystallization solvent, the recrystallization temperature and the like, the purity of the enamine salt is improved by 4-6%, the purity of the finished product can reach 99% at most, the yield of the recrystallized product is improved by 28%, and the recrystallization yield can reach 95% atmost; and the method is simple to operate and low in cost, an efficient way is provided for purification of enamine salt, and the yield of the VB1 intermediate thiothiamine is effectively increased.

Description

technical field [0001] The invention belongs to the technical field of compound purification, in particular to an enamine salt recrystallization purification method. Background technique [0002] Enamine salt is an important chemical intermediate, which is widely used in the fields of medicine and pesticide. At present, the enamine salt is generally prepared by chlorination of sodium salt as raw material, but the purity of the enamine salt prepared by this method is generally 90-98%, and its impurity content is 2-10%, which severely limits its application. [0003] At present, there are few reports on the purification of enamine salts. Therefore, it is necessary to find a simple, effective, and low-cost purification method for enamine salts. Contents of the invention [0004] The technical problem to be solved by the present invention is to provide a simple, effective, and low-cost enamine salt purification method. [0005] The technical solution adopted by the present i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D9/02
CPCB01D9/00
Inventor 王文杨梓剑王淑霞朱庆林郑玲艳
Owner 内蒙古益泽制药有限公司