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A kind of enamine salt recrystallization purification method

A purification method and enamine salt technology, applied in chemical instruments and methods, crystallization separation, separation methods, etc., can solve problems such as limited applications, and achieve the effects of low cost, high recrystallization efficiency, and high feasibility

Active Publication Date: 2022-04-05
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 a method for recrystallization and purification of enamine salt, which comprises the following steps: mixing the crude product of enamine salt with methanol solvent at a solid-to-liquid mass ratio of 1:1-5, heating until all the solids are dissolved, and cooling to 5-5. At 30°C, crystallize, filter, and dry to obtain the finished product of enamine salt. The method of the invention improves the purity of the enamine salt by 4-6% through the control of parameters such as the selection of the recrystallization solvent and its dosage, and the recrystallization temperature, the purity of the finished product can reach up to 99%, and the yield of the recrystallization product is increased by 28%. . The recrystallization yield can reach up to 95%. This method is easy to operate and low in cost, provides an efficient way for the purification of enamine salts, and effectively improves the yield of VB1 intermediate thiothiamine.

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 Patents(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