Novel method for synthesizing vitamin B1 hydrochloride

A vitamin and hydrochloride technology, applied in the direction of organic chemistry, can solve the problems of high toxicity of barium chloride, difficult implementation, and difficult removal of ammonium chloride, and achieve the effect of environmental friendliness and simplified production process

Inactive Publication Date: 2013-03-06
HUAZHONG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] Although the patent "Preparation of vitamin B with thiol thiamine 1 A new method of hydrochloride" (patent application number: 02109717.8) describes the use of barium chloride to treat vitamin B 1 Sulfate in sulfate, but: 1, barium chloride is too toxic to be implemented in industrial production; 2, ammonium chloride generated when ammonium bicarbonate is used to remove excess barium chloride is not easy to remove
Therefore, the process of this patent cannot be used in process production

Method used

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  • Novel method for synthesizing vitamin B1 hydrochloride
  • Novel method for synthesizing vitamin B1 hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] time w / w%SO 4 2- 0.5h 3.5 1.5h 0.5 2.5h 0.25 3.0h 0.01

[0023] The resin was filtered off, washed with 100 g of purified water, and the filtrate (90 g) and washings (90 g) were analyzed separately. Analyze sulfate content and thiamine hydrochloride content.

[0024] w / w% Thiamine Hydrochloride 22.000 w / w%SO 4 2- 0.010 w / w% yield 90.000

[0025] w / w% Thiamine Hydrochloride 2.100 w / w%SO 4 2- 0.001 w / w% yield 8.690

[0026] Combine the filtrate and washing liquid and add them to a rotary evaporator to concentrate until some substances are precipitated, then add 200g of ethanol, cool down to 0°C, let it crystallize completely, filter, and dry to obtain 20.5g of vitamin B 1 Hydrochloride. The analytical content is 99.9 w / w %, sulfate, nitrate, absorption and other indicators are qualified.

[0027] The resin was regenerated with 1000 g of aqueous sodium hydroxide solution ...

Embodiment 2

[0029] Continuous process:

[0030] At 25°C, 400ml of wet resin 330 (cl - type) into the column, wash the resin with 1500g sodium hydroxide aqueous solution (4 w / w %), flow rate: m / h 4, contact time: minute: 60; then wash with pure water until neutral, flow rate: m / h h 15, time: minute: about 30; then wash the resin with 1500g hydrochloric acid aqueous solution (4 w / w %), flow rate: m / h 4, contact time: minute: 60; then wash with pure water until neutral, flow rate: m / h 15, time: minute: about 30; repeat washing like this for 3 luns, wash off the impurities in the new resin, and use sodium hydroxide solution for the last time, thus preparing the resin as OH - Form pillars.

[0031] Use hydrochloric acid to adjust 2000ml of thiamine sulfate aqueous solution (sulfate root 7.06w / w%, thiamine 17.8w / w%) to adjust pH=1.5, then load it on the column at a flow rate of 3.45ml, and collect at a flow rate of 400ml / h The eluent, counted as 100ml each time, was collected 21 times afte...

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PUM

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Abstract

The invention provides a novel method for synthesizing a vitamin B1 hydrochloride. The method comprises the following steps of: treating a vitamin B1 sulfate aqueous solution by adopting an ion exchange resin; removing sulfate radicals; and concentrating and crystalizing to prepare the vitamin B1 hydrochloride. Due to the adoption of the method, the conventional process for producing a vitamin B1 hydrochloride by transforming from thiamine mononitrate is eliminated, residues of an organic solvent in a product are avoided since an organic solvent is not adopted, a process for preparing acid methanol from hydrochloric acid gas by using chlorosulfonic acid is eliminated simultaneously, and environmental pollution is lowered.

Description

technical field [0001] The present invention relates to a pharmaceutical method, in particular to a method for treating vitamin B with ion exchange resins. 1 Sulfate solution is processed to produce vitamin B 1 HCl method. Background technique [0002] Vitamin B 1 Hydrochloride, referred to as VB 1 Hydrochloride, synonym: thiamine hydrochloride, thiamine hydrochloride; [0003] Chemical name: 3-(4-amino-2-methyl-5-pyrimidinyl)methyl-5-(β-hydroxyethyl)-4-methylthiazole chloride hydrochloride; [0004] Structural formula: [0005] [0006] Existing industrial production of vitamin B 1 Hydrochloride, generally using vitamin B 1 Nitrates and B vitamins 1 The difference in the solubility of sulfate in water, the vitamin B 1 Sulfate first converts to vitamin B 1 Nitrate is precipitated, and then converted into vitamin B with hydrogen chloride gas methanol solution 1 Hydrochloride. [0007] However, what this process uses is hydrochloric acid, and what generates is n...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D417/06
Inventor 王勇李新宇付林王英薛俊徐勇
Owner HUAZHONG PHARMA
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