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Refining method of thiothiamine and the obtained thiothiamine product and vitamin B1 product

A technology of thiothiamine and refining method, which is applied in the field of thiothiamine products and vitamin B1 products, and can solve the problems of vitamin B1 product rework, vitamin B1 production cost increase, vitamin B1 chromatographic purity and other detection indicators unqualified, etc. problems, to achieve the effect of increased purity

Active Publication Date: 2021-11-23
江苏兄弟维生素有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Thiothiamine is used as an intermediate in the synthesis of vitamin B1. The content of thiothiamine synthesized by the current technology can only reach 90% to 95%, and these thiothiamine containing 5% to 10% of impurities are very important for the later preparation The quality of vitamin B1 has a great influence, which can easily lead to unqualified detection indicators such as chromatographic purity of vitamin B1, and even lead to rework of vitamin B1 products in serious cases, resulting in an increase in the production cost of vitamin B1

Method used

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  • Refining method of thiothiamine and the obtained thiothiamine product and vitamin B1 product
  • Refining method of thiothiamine and the obtained thiothiamine product and vitamin B1 product

Examples

Experimental program
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Effect test

Embodiment 1

[0082] A refined method for thiothiamine, said method comprising the following steps:

[0083] (1), first wash the crude thiothiamine with ethanol at 15° C. to remove impurities soluble in ethanol in the crude thiothiamine, then filter and dry to obtain the crude thiothiamine after alcohol washing ;

[0084] The ratio of the thiothiamine crude product to ethanol is 1:2.

[0085] The drying time after the alcohol washing is 2 hours, and the temperature is 40°C;

[0086] (2) The crude thiothiamine washed with alcohol and dried was washed with distilled water at 15° C. to remove impurities dissolved in water in the thiothiamine to obtain crude product A;

[0087] The ratio of the crude thiothiamine to distilled water is 1:2.

[0088] The drying time after washing with water is 5 hours, and the temperature is 60°C;

[0089] (3) Mix the crude product A and ethanol at a ratio of 1:40, then reflux and heat up to 70°C until the crude product A is completely dissolved to obtain sol...

Embodiment 2

[0094] A refined method for thiothiamine, said method comprising the following steps:

[0095] (1), first wash the crude thiothiamine with ethanol at 25° C. to remove impurities soluble in ethanol in the crude thiothiamine, then filter and dry to obtain the crude thiothiamine after alcohol washing ;

[0096] The ratio of the thiothiamine crude product to ethanol is 1:5.

[0097] The drying time after the alcohol washing is 5 hours, and the temperature is 50°C;

[0098] (2) The crude thiothiamine washed with alcohol and dried was washed with distilled water at 25° C. to remove impurities dissolved in water in the thiothiamine to obtain crude product A;

[0099] The ratio of the crude thiothiamine to distilled water is 1:5.

[0100] The drying time after washing with water is 8 hours, and the temperature is 80°C;

[0101] (3) Mix the crude product A and ethanol at a ratio of 1:60, then reflux and heat up to 80°C until the crude product A is completely dissolved to obtain sol...

Embodiment 3

[0106] A refined method for thiothiamine, said method comprising the following steps:

[0107] (1), first wash the crude thiothiamine with ethanol at 18°C ​​to remove impurities soluble in ethanol in the crude thiothiamine, then filter and dry to obtain the crude thiothiamine after alcohol washing ;

[0108] The ratio of the thiothiamine crude product to ethanol is 1:3.

[0109] The drying time after the alcohol washing is 3 hours, and the temperature is 42°C;

[0110] (2) The crude product of thiothiamine washed with alcohol and dried was washed with distilled water at 18° C. to remove impurities dissolved in water in the thiothiamine to obtain crude product A;

[0111] The ratio of the crude thiothiamine to distilled water is 1:4.

[0112] The drying time after washing with water is 6 hours, and the temperature is 65°C;

[0113] (3) Mix crude product A and ethanol at a ratio of 1:55, then reflux and heat up to 78°C until crude product A is completely dissolved to obtain ...

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Abstract

The invention provides a method for refining thiothiamine and the resulting thiothiamine product and vitamin B1 product, and relates to the technical field of compound purification. The method firstly washes the crude product of thiothiamine with alcohol and water to obtain crude product A; then dissolves the crude product A in low-carbon alcohol to obtain solution A, and decolorizes to obtain solution B; then the thiothiamine is obtained from the solution Precipitate in B and dry to obtain refined thiothiamine. It is detected that the purity of the refined thiothiamine in the present invention can be significantly improved compared with the thiothiamine synthesized by the existing technology, which provides guarantee for the preparation of subsequent vitamin B1 products.

Description

technical field [0001] The invention relates to the technical field of compound purification, in particular to a method for refining thiothiamine and the resulting thiothiamine product and vitamin B1 product. Background technique [0002] Thiothiamine is used as an intermediate in the synthesis of vitamin B1. The content of thiothiamine synthesized by the current technology can only reach 90% to 95%, and these thiothiamine containing 5% to 10% of impurities are very important for the later preparation The quality of vitamin B1 has a great impact, which can easily lead to unqualified detection indicators such as chromatographic purity of vitamin B1. In severe cases, it may even lead to rework of vitamin B1 products, resulting in an increase in the production cost of vitamin B1. [0003] In view of this, the present invention is proposed. Contents of the invention [0004] The first object of the present invention is to provide a kind of refining method of thiothiamine, des...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D417/06
CPCC07D417/06
Inventor 李褦成陈英明张杰许凡
Owner 江苏兄弟维生素有限公司
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