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Preparation of piperaquini phosphatis

A technology of piperaquine phosphate and quinoline, which is applied in the field of preparation of raw materials, can solve the problems of large environmental pollution, high production cost, and low product yield, and achieve low environmental pollution, low production cost, and high product yield. Effect

Active Publication Date: 2009-05-27
CHONGQING KANGLE PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above three preparation methods all have the disadvantages of low product yield, large environmental pollution and high production cost.

Method used

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  • Preparation of piperaquini phosphatis
  • Preparation of piperaquini phosphatis
  • Preparation of piperaquini phosphatis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Embodiment 1, the preparation of piperaquine phosphate

[0022] Include the following steps:

[0023] The preparation of a, 7-chloro-4-(1-piperazinyl) quinoline

[0024] According to the theoretical production amount of 7-chloro-4-(1-piperazinyl) quinoline 74.3g, calculate the amount of raw materials; in a 2000mL three-necked round-bottomed flask, add 4,7-dichloroquinoline 59.4g (0.3mol), Anhydrous piperazine 206.4g (2.4mol) and potassium carbonate 41.4g (0.3mol), then add water 600mL, reflux reaction 36 hours, monitor reaction progress with thin-layer chromatography (TLC) method, after the reaction is complete, the reaction solution Distilled under reduced pressure to 1 / 2 volume, extracted 3 times with 600 mL of ethyl acetate, collected and combined the ethyl acetate extracts, concentrated, and dried under vacuum at 55°C to obtain 7-chloro-4-(1-piperazinyl ) quinoline 72.8g, purity 98.5%, yield 98.0%;

[0025] b, the preparation of piperaquine

[0026] Calculate th...

Embodiment 2

[0030] Embodiment 2, the preparation of piperaquine phosphate

[0031] Include the following steps:

[0032] The preparation of a, 7-chloro-4-(1-piperazinyl) quinoline

[0033] According to the theoretical production amount of 7-chloro-4-(1-piperazinyl) quinoline 74.3g, calculate the amount of raw materials; in a 2000mL three-necked round-bottomed flask, add 4,7-dichloroquinoline 59.4g (0.3mol), Anhydrous piperazine 258g (3mol) and salt of wormwood 41.4g (0.3mol), add methanol 600mL again, reflux reaction 36 hours, monitor the progress of reaction with TLC method, after the reaction is complete, the reaction solution is distilled off under reduced pressure to remove methanol, and then Add 300 mL of water, extract with 600 mL of dichloromethane for 3 times, collect and combine the dichloromethane extracts, concentrate, and dry under vacuum at 55°C to obtain 73.2 g of 7-chloro-4-(1-piperazinyl)quinoline, Purity 99.2%, yield 98.5%;

[0034] b, the preparation of piperaquine

...

Embodiment 3

[0039] Embodiment 3, the preparation of piperaquine phosphate

[0040] Include the following steps:

[0041] The preparation of a, 7-chloro-4-(1-piperazinyl) quinoline

[0042] According to the theoretical production amount of 7-chloro-4-(1-piperazinyl) quinoline 74.3g, calculate the amount of raw materials; in a 2000mL three-necked round-bottomed flask, add 4,7-dichloroquinoline 59.4g (0.3mol), Anhydrous piperazine 309.6g (2.6mol) and potassium carbonate 41.4g (0.3mol), then add propanol 600mL, reflux reaction for 36 hours, monitor the progress of the reaction with TLC method, after the reaction is complete, the reaction solution is distilled off under reduced pressure Propanol, then add 300mL of water, extract with 600mL of ethyl acetate three times, collect and combine the ethyl acetate extracts, concentrate, and dry under vacuum at 55°C to obtain 7-chloro-4-(1-piperazinyl)quinone 74.0g of morphine, with a purity of 98.4%, and a yield of 99.6%;

[0043] b, the preparation ...

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Abstract

The invention discloses a method for preparing piperaquine phosphate. 4,7-dichloroquinoline is taken as an initial raw material and is subjected to condensation reaction with anhydrous piperazidine first to obtain 7-chloro-4-(1-piperazinyl)quinoline, then the 7-chloro-4-(1-piperazinyl)quinoline is subjected to condensation reaction with 1, 3-bromochloropropane to obtain piperaquine, and finally the piperaquine is salified with phosphorous acid to obtain the piperaquine phosphate. The method has a simple process, is easy to purify intermediate products and a final product, has high product yield and good quality, avoids the use of toxic reagents, has small pollution to the environment and low production cost, and is suitable for industrialized production.

Description

technical field [0001] The present invention relates to a kind of preparation method of crude drug, particularly a kind of preparation method of piperaquine phosphate. Background technique [0002] Today, malaria is still listed as the world's three major catastrophic diseases together with AIDS and tuberculosis, and more than 90 countries and regions are still in the middle and high prevalence levels of malaria. According to the statistics of the World Health Organization (WHO), there are 300-500 million malaria-infected people in the world every year, and the death toll exceeds 1 million, and most of them are children under the age of five. In order to enhance the therapeutic effect and slow down the occurrence of drug resistance, since 2001, WHO has recommended the use of "Artemesinin-based Combination Therapy (ACT)" for the treatment of malaria. Piperaquine phosphate is a synthetic antimalarial drug, mainly used in the treatment of malaria resistant to chloroquine. In ...

Claims

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Application Information

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IPC IPC(8): C07D215/42
Inventor 杨继斌余毅王建波张宇生
Owner CHONGQING KANGLE PHARMA
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