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Preparation method of thiamine hydrochloride, thiamine hydrochloride, application of thiamine hydrochloride and vitamin B1

A technology of thiamine hydrochloride and vitamins, applied in the direction of organic chemistry, etc., to achieve the effect of optimizing the synthesis process route, reducing the content, and broadening the application field

Pending Publication Date: 2022-03-15
江苏兄弟维生素有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] One of the purposes of the present invention is to provide a preparation method of thiamine hydrochloride, which aims to solve the technical problem that the existing preparation method is prone to produce by-product oxythiamine, and improve the quality of thiamine hydrochloride

Method used

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  • Preparation method of thiamine hydrochloride, thiamine hydrochloride, application of thiamine hydrochloride and vitamin B1
  • Preparation method of thiamine hydrochloride, thiamine hydrochloride, application of thiamine hydrochloride and vitamin B1
  • Preparation method of thiamine hydrochloride, thiamine hydrochloride, application of thiamine hydrochloride and vitamin B1

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preparation example Construction

[0037] A kind of preparation method of thiamine hydrochloride provided according to the first aspect of the present invention comprises the following steps:

[0038] Step A: neutralizing the mother liquor of thiamine sulfate to obtain a neutralizing solution;

[0039] Step B: adding ammonium nitrate solution to the neutralizing solution and then filtering to obtain thiamine nitrate and thiamine sulfate mother liquors;

[0040] Step C: repeat the operation of steps A-B to the thiamine sulfate mother liquor that step B obtains;

[0041] Step D: converting the thiamine nitrate to obtain the thiamine hydrochloride.

[0042] The preparation method of thiamine hydrochloride provided by the invention, the preparation method is by controlling the synthesis process of intermediate thiamine nitrate, because the by-product is produced in the later stage of salt conversion, so the neutralization and conversion of salt is carried out many times, reducing the content of by-products, making...

Embodiment 1

[0081] The present embodiment provides a kind of preparation technology of thiamine hydrochloride, such as figure 1 As shown, it specifically includes the following steps:

[0082] (1) Take 238g of thiamine sulfate solution (the concentration of thiamine sulfate is about 30%), add 14wt.% ammonia water dropwise, pre-adjust the pH to 5.85, and keep the temperature within the range of 8-15°C.

[0083] (2) A small amount of thiamine nitrate crystals were added as seed crystals, stirred for 15 minutes, and about 24 g of 50 wt.% ammonium nitrate solution was added dropwise at a rate of 0.4 g / min to perform a salt conversion reaction.

[0084] (3) After the dropwise addition, ammonia water was added dropwise, the pH was adjusted to 7.3, and the temperature was lowered to 10° C. for filtration. The obtained wet thiamine nitrate and mother liquor were dried at 60° C.

[0085] (4) Repeat above-mentioned steps (1)-(3) with mother liquor, carry out secondary salt conversion, obtain the t...

Embodiment 2

[0088] The present embodiment provides a kind of preparation technology of thiamine hydrochloride, and the difference with embodiment 1 is, the add-on of ammonium nitrate solution is 30g in the step (2), and the add-on of ammonium nitrate solution in the step (4) is 18g, and the rest The steps and raw materials are the same as those in Example 1, and will not be repeated here.

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Abstract

The invention provides a preparation method of thiamine hydrochloride, thiamine hydrochloride, application of thiamine hydrochloride and vitamin B1, and relates to the technical field of compound preparation. The preparation method comprises the following steps: step A, neutralizing a thiamine sulfate mother solution to obtain a neutralized solution; step B, adding an ammonium nitrate solution into the neutralization solution, and filtering to obtain thiamine nitrate and thiamine sulfate mother liquor; c, repeating the operation of the steps A-B on the thiamine sulfate mother liquor obtained in the step B; and step D, carrying out salt conversion on the thiamine nitrate to obtain the thiamine hydrochloride. According to the preparation method, the synthesis is carried out towards the process of generating thiamine nitrate by controlling the synthesis process of an intermediate thiamine nitrate and carrying out small-amount and multiple-time neutralization and salt conversion, so that the quality of thiamine nitrate is improved, the content of an impurity D is reduced, medicinal thiamine hydrochloride can be generated, and the synthesis process route of thiamine hydrochloride is optimized; and the method has very important influence on the product quality and economic benefit of thiamine hydrochloride production.

Description

technical field [0001] The invention relates to the technical field of compound preparation, in particular to a preparation method of thiamine hydrochloride, thiamine hydrochloride and its application and vitamin B1. Background technique [0002] Thiamine hydrochloride, vitamin B1 hydrochloride, chemical name is 3-[(4-amino-2-methyl-5-pyrimidinyl)methyl]-5-(2-hydroxyethyl)-4-methyl Thiazole hydrochloride has a structural formula as shown in the following formula (1). In the body, vitamin B1 participates in the catabolism of sugar in the form of a coenzyme, protects the nervous system, promotes gastrointestinal motility, and increases appetite. It is widely used in clinical and breeding. [0003] [0004] Thiamine hydrochloride is produced through the conversion of intermediate thiamine nitrate to salt. The current preparation method of intermediate thiamine nitrate will produce by-product oxothiamine (impurity D), which will affect the quality of thiamine hydrochloride....

Claims

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Application Information

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IPC IPC(8): C07D415/00
CPCC07D415/00
Inventor 冯云琪严建斌陈英明郭军军段艳文
Owner 江苏兄弟维生素有限公司
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