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Production of primaquine phosphate

A technology of primaquine phosphate and pickling, applied in the direction of organic chemistry, etc., can solve the problems of low content index of primaquine phosphate and the like

Inactive Publication Date: 2007-09-05
常熟市南湖实业化工厂
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The content index of the above-mentioned primaquine phosphate is relatively low, and there is no requirement for related substances such as 8-aminoquinoline

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Condensation reaction: Add 35kg of amino substances, 12kg of soda ash and 37kg of condensates (content ≥ 80%) in the reaction pot, heat to 58°C, keep warm for 20min to dissolve all the materials, start stirring, continue to heat up to 147°C, keep warm for 8h , the whole reaction is in the empty state, the reaction is over, suck the material into the dilution pot while it is hot, put 140kg of toluene in the dilution pot in advance, after the material is sucked, add 100kg of toluene, stir evenly, about 15min, filter, and the filtrate is sucked into the pickling pot , discard the filter residue, add 500kg of sulfuric acid with a concentration of 30% into the pickling pot, slowly raise the temperature to 75-80°C, let it stand for 0.5h, separate the water layer, and wash the separated material liquid with water for many times to wash away the acidity , move the feed liquid into the distillation pot, steam the toluene at normal pressure, raise the temperature to 130°C, reduce ...

Embodiment 2

[0025] Condensation reaction: Add 35kg of amino substances, 12kg of soda ash and 37kg of condensate (content ≥ 80%) in the reaction pot, heat to 59°C, keep warm for 18min, dissolve all the materials, start stirring, continue to heat up to 149°C, keep warm for 7.5 h, the whole reaction is in the empty state, the reaction is over, suck the material into the dilution pot while it is hot, put 140kg of toluene in the dilution pot in advance, after the material is sucked, add 100kg of toluene, stir evenly, about 12min, filter, and the filtrate is picked up by pickling pot, discard the filter residue, add 500kg of sulfuric acid with a concentration of 30% to the pickling pot, slowly raise the temperature to 75-80°C, let it stand for 0.4h, separate the water layer, and rinse the separated material liquid with water for many times, wash away Acidity, move the feed liquid into the distillation pot, steam the toluene at normal pressure, raise the temperature to 132°C, reduce the pressure ...

Embodiment 3

[0029]Condensation reaction: Add 35kg of amino substances, 12kg of soda ash and 37kg of condensates (content ≥ 80%) in the reaction pot, heat to 60°C, keep warm for 19min to dissolve all the materials, start stirring, continue to heat up to 150°C, and keep warm for 7h , the whole reaction is in the empty state, the reaction is over, suck the material into the dilution pot while it is hot, put 140kg of toluene in the dilution pot in advance, after the material is sucked, add 100kg of toluene, stir evenly, about 8min, filter, and the filtrate is sucked into the pickling pot , discard the filter residue, add 500kg of sulfuric acid with a concentration of 30% to the pickling pot, slowly raise the temperature to 75-80°C, let it stand for 0.45h, separate the water layer, and wash the separated material liquid with water for many times to wash away the acidity , move the feed liquid into the distillation pot, steam the toluene at normal pressure, raise the temperature to 133°C, reduce...

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PUM

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Abstract

A process for preparing primaquine phosphate includes such steps as adding amino compound, sodium carbonate and monocondensate in reactor, condensation reaction to obtain dicondensate, mixing it with methanol and hydrazine hydrate, cyclizing reaction to obtain the mixture of primaquine and solvent, mixing it with water, alcohol and phosphoric acid, crystallizing reaction, and pulverizing.

Description

technical field [0001] The invention relates to a preparation method of primaquine phosphate, which is an improvement on the prior preparation method of primaquine phosphate, and belongs to the technical field of preparation of quinoline drugs. Background technique [0002] Primaquine phosphate is orange-red crystalline powder, odorless, bitter, soluble in water but insoluble in chloroform and ether, its chemical name is: N4-(6-methoxy-8-quinolyl)-1- Pentamethylene diamine diphosphate, the molecular formula is: C 15 h 21 N 3 Oh 3 PO 4 , the molecular weight is 455.34. Because it has a strong killing effect on the extraerythrocytic stage of Plasmodium vivax and the gametocytes of various Plasmodium parasites, it is called an antimalarial drug in the industry, and it is included in the "China High-tech Product Catalogue" (2006) [5] middle. [0003] Literature search shows that: China Shanghai Zhongxi Pharmaceutical Co., Ltd., Changshu Lianchuang Chemical Co., Ltd., Jian...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D215/40
Inventor 陆永林
Owner 常熟市南湖实业化工厂