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Preparation process of chloroquine phosphate

A chloroquine phosphate and preparation technology, which is applied in the field of medicine and chemical industry, can solve the problems of being unfriendly to the human body and the environment, low production efficiency, high process energy consumption, etc., and achieve the effects of simple operation, improved production efficiency and high product purity

Active Publication Date: 2020-09-15
JINGHUA PHARMA GRP NANTONG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At the same time, the detection of benzene residues in the finished product should also be considered. There are problems such as high process energy consumption, cumbersome operation, low production efficiency, and unfriendly to human body and environment.

Method used

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  • Preparation process of chloroquine phosphate
  • Preparation process of chloroquine phosphate
  • Preparation process of chloroquine phosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Add 30 g of 4,7-dichloroquinoline and 24 g of 2-amino-5-diethylaminopentane into a three-necked round-bottomed flask, stir to raise the temperature, keep the reaction at 135°C-140°C for more than 24 hours, and determine the end point of the reaction by HPLC detection. Cool down to about 100°C, add 75g of 6% NaOH solution, measure the pH value of about 11-12, continue to cool down to about 40°C, add 90g of dichloromethane, stir and stand for stratification, collect the organic layer, and use dichloromethane for the water layer 54g was extracted twice, and the organic layers were combined and washed three times with 120g of water. The organic layer was evaporated to dryness in a water bath at 65 °C under reduced pressure, 200 g of isopropyl ether was added, stirred and crystallized at -5 °C to 0 °C for 3 h, and suction filtered to obtain a khaki solid with a wet weight of 43.5 g. Air-dried at 50°C to obtain 35.0 g of dry product with a yield of 72.34%.

[0043] Salt form...

Embodiment 2

[0046]Condensation: Add 50g of 4,7-dichloroquinoline and 50g of 2-amino-5-diethylaminopentane into a three-neck round-bottomed flask, stir and raise the temperature, keep the temperature at 135℃~140℃ for more than 24h, and judge the end point of the reaction by HPLC detection . Cool down to about 100°C, add 125g of 6% NaOH solution, measure the pH value of about 11-12, continue to cool down to about 40°C, add 150g of dichloromethane, stir and stand for stratification, collect the organic layer, and use dichloromethane for the water layer 90g was extracted twice, and the organic layers were combined and washed three times with 200g of water. The organic layer was evaporated to dryness in a water bath at 65°C under reduced pressure, 200g of isopropyl ether was added, stirred and crystallized at 0-5°C for 3h, and suction filtered to obtain a khaki solid with a wet weight of 73g. Air-dried at 50°C to obtain 58.5 g of dry product with a yield of 72.44%.

[0047] Salt formation: a...

Embodiment 3

[0050] Condensation: Add 50g of 4,7-dichloroquinoline and 60g of 2-amino-5-diethylaminopentane into a three-neck round bottom flask, stir and raise the temperature, keep it at 135℃~140℃ for more than 24h, and judge the end point of the reaction by HPLC detection . Cool down to about 100°C, add 125g of 6% NaOH solution, measure the pH value of about 11-12, continue to cool down to about 40°C, add 150g of dichloromethane, stir and stand for stratification, collect the organic layer, and use dichloromethane for the water layer 90g was extracted twice, and the organic layers were combined and washed three times with 200g of water. The organic layer was evaporated to dryness in a water bath at 65 °C under reduced pressure, 200 g of isopropyl ether was added, stirred and crystallized at -5 °C to 0 °C for 3 h, and suction filtered to obtain a khaki solid with a wet weight of 80 g. Air-dried at 50°C to obtain 64.5 g of dry product with a yield of 79.88%.

[0051] Salt formation: add...

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Abstract

The invention discloses a preparation process of chloroquine phosphate. The preparation process of the chloroquine phosphate comprises the following steps of: (1) taking 4, 7-dichloroquinoline as an initial raw material, carrying out condensation reaction with 2-amino-5-diethylaminopentane, and carrying out alkalization extraction to obtain chloroquine; and (2) salifying the chloroquine obtained in the step (1) with phosphoric acid to obtain chloroquine phosphate. The invention provides a preparation process of chloroquine phosphate. In the preparation process, the use of organic solvents suchas benzene and other catalysts such as phenol is avoided, and a condensation crystallization impurity removal step is introduced, so that the product purity is high, the individual impurity is less than 0.1%, the green chemical requirements and pharmacopeia standards are met, the operation is simple and convenient, the process is simplified, the production efficiency is improved, and the method is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of medicine and chemical industry, and in particular relates to a preparation process of chloroquine phosphate. Background technique [0002] Chloroquine Phosphate (Chloroquine Phosphate), chemical name N', N'-diethyl-N4-(7-chloro-4-quinolyl)-1,4-pentanediamine diphosphate, used to treat sensitivity to chloroquine falciparum, vivax and other malaria. It can also be used for the treatment of parenteral amoebiasis, as well as anti-rheumatic effects. According to research, the drug can effectively inhibit the infection of the new coronavirus 2019-nCoV at the cellular level. [0003] In the previously disclosed preparation method of chloroquine phosphate, the raw materials used are 4,7-dichloroquinoline benzene solution, an equal amount of solvent and catalyst phenol, and 2-amino-5-diethylaminopentane. The specific process is to remove benzene from the 4,7-dichloroquinoline benzene solution under normal press...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D215/46
CPCC07D215/46Y02A50/30
Inventor 滕飞袁拥军吴玉祥李淑芬顾建波
Owner JINGHUA PHARMA GRP NANTONG
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