Producing method of of tranexamic acid

A technology of tranexamic acid and its production method, which is applied in the field of production of tranexamic acid, can solve the problem that the quality does not meet the Chinese Pharmacopoeia 2000 edition, the British Pharmacopoeia 93 edition, the Japanese Pharmacopoeia 13 edition, the unit yield, that is, the labor productivity is not high, Long conversion reaction time and other problems, to achieve the effect of reducing raw material consumption, shortening conversion reaction time, and improving labor production efficiency

Inactive Publication Date: 2004-09-01
HUNAN DONGTING PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In a word, so far, the production methods of tranexamic acid both at home and abroad have a cis-isomer content of more than 0.5% no matter the method A or method B, and its quality has not reached the Chinese Pharmacopoeia 2000 edition, the British Pharmacopoeia 93 edition, and the Japanese Pharmacopoeia Bureau. The 13th edition and the European Pharmacopoeia 2000 editio

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] ①, catalytic hydrogenation

[0031] Add 15 kg of p-carboxybenzylamine and 495 liters of water into the reaction tank, add 8.4 liters of sulfuric acid under stirring, heat to dissolve; add 0.75 kg of platinum dioxide (add water to fully moisten it first); remove the air in the tank and then pass hydrogen to react: Temperature 38°C, pressure 0.08Mpa, react until the hydrogen absorption reaches the theoretical amount and stop absorbing hydrogen; remove the residual hydrogen, filter the reaction solution, wash platinum black (recycle); heat the filtrate to 90°C, add barium carbonate to neutralize to PH7.3; after standing still, filter barium sulfate; wash the filter residue with water, merge the filter and lotion, and after concentrating, get 50 liters of cis liquid of p-aminomethylcyclohexanecarboxylic acid (concentration is every 10 mol p-Carboxybenzylamine reaction solution was concentrated to 5 L).

[0032] ②, conversion crystallization

[0033] Add the above 50 liter...

Embodiment 2

[0035] ①, catalytic hydrogenation

[0036] The process steps are the same as in Example 1, except that some technical parameters are different: the reaction temperature is 42°C, and the pressure is 0.12Mpa; add barium carbonate to neutralize to PH7.

[0037] ②, conversion crystallization

[0038] The process steps are the same as in Example 1, except that some technical parameters are different: 60 kilograms of barium hydroxide are added; the temperature is raised to 255° C., the pressure is 4.3 Mpa, and the reaction time is 9 hours; 120 liters of water are added after the reaction, and the temperature is raised to 65° C.; and to PH6.1; adjust to PH5.4 with sulfuric acid; stand for 6 hours, wash the filter cake with 25 liters of water; add 1 kg of activated carbon; dry the filter cake to obtain 9.2 kg of tranexamic acid, with a one-way yield of 61.33%, cis Content 0.15%.

Embodiment 3

[0039] Embodiment 3 (best)

[0040] ①, catalytic hydrogenation

[0041] The process steps are the same as in Example 1, except that some technical parameters are different: the reaction temperature is 40°C, and the pressure is 0.1Mpa; add barium carbonate to neutralize to PH7.

[0042] ②, conversion crystallization

[0043] The process steps are the same as in Example 1, except that some technical parameters are different: 40 kg of barium hydroxide is added; the temperature is raised to 250°C, the pressure is 4Mpa, and the reaction time is 8 hours; 100 liters of water is added after the reaction, and the temperature is raised to 60°C; neutralized with carbon dioxide Adjust pH to 6.5 with sulfuric acid; leave for 7 hours: wash the filter cake with 40 liters of water: add 1.2 kg of activated carbon: add 80 liters of ethanol for crystallization: cool to 10°C; wash the crystallization with 20 liters of ethanol; dry the filter cake 9.8 kg of tranexamic acid was obtained with a on...

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PUM

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Abstract

The invention discloses a process for producing tranexamic acid, wherein p-aminomethyl benzoic acid raw material is hydrogenised, and the hydrogenization liquid is neutralized to pH7-7.5 through barium carbonate, after filtering, the solution is condensed to 10 gram molecule p-aminomethyl benzoic acid reaction liquid of 5l, then charge raw materials by the portion ratio of ammonia cyclohexyl-methane carboxyl acid sym-form liquid (V) : barium hydroxide (W) : water (W) : ethanol (V) = 1:0.5-1.5:2-3.5:1.5-3, elevating the temperature to 230-260 deg. C, the pressure being 2.9-4.8.0Mpa, reacting time being 7.5-10 hours, after reaction charging water and elevating the temperature to 60-70 deg. C, neutralizing through carbon dioxide till pH=6-7.5, filtering and adjusting pH=5.2-5.5 through sulfuric acid, stewing, charging right amount activated charcoal, boiling and decolorizing, filtering, filter cake washing, condensing, charging ethanol for recrystallization, cooling down to 8-12 deg. C, filtering, washing crystallization by ethanol, filter cake drying to obtain tranexamic acid.

Description

technical field [0001] The invention relates to a production method of tranexamic acid (also known as tranexamic acid). Background technique [0002] For many years, the production methods of tranexamic acid in China have two methods: method A, namely the methyl acrylate method and method B, namely the p-carboxybenzylamine method. In 1980, the "National Compendium of Raw Materials and Processes" edited by the State Administration of Medicine published P510-512 The operating standards are given on the page. [0003] Method A was originally used by Shanghai, Jiangsu and other manufacturers. Because this method uses highly toxic cyanide banned by the state as raw material, it has basically stopped using it at present. [0004] The production steps and process conditions of method B are as follows: [0005] ①, catalytic hydrogenation [0006] Ingredients ratio p-carboxybenzylamine (W): platinum dioxide (W): sulfuric acid (V): water (V) = 1: 0.05: 0.56: 33 ...

Claims

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Application Information

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IPC IPC(8): C07C227/16C07C229/38
Inventor 叶云付王迪凡
Owner HUNAN DONGTING PHARMA
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