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Method for synthesizing piperaquine intermediate in continuous flow microreactor

An intermediate, piperaquine technology, applied in the field of synthesis of intermediate 7-chloro-4-quinoline, can solve the problems of low yield and poor purity, and achieve high yield, short processing flow and few by-products Effect

Inactive Publication Date: 2019-07-05
CHONGQING KANGLE PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] In order to solve problems such as low yield and poor purity in traditional synthetic reactions, the object of the invention is to overcome the deficiencies in the prior art, and provide a continuous flow microreactor for the synthesis of piperaquine phosphate key intermediate 7-chloro-4-( 1-piperazinyl)quinoline

Method used

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  • Method for synthesizing piperaquine intermediate in continuous flow microreactor
  • Method for synthesizing piperaquine intermediate in continuous flow microreactor
  • Method for synthesizing piperaquine intermediate in continuous flow microreactor

Examples

Experimental program
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Effect test

Embodiment 1

[0028] This embodiment provides a method for utilizing a microchannel reactor to synthesize piperaquine phosphate key intermediate 7-chloro-4-(1-piperazinyl)quinoline, and the synthetic method is as follows:

[0029] (1) take by weighing 198g4, the dichloromethane that 7-dichloroquinoline adds 594g, after stirring, fully stir and mix to dissolving clear formation material I, material I is delivered to the preheating module of microchannel reactor and carries out preheating;

[0030] (2) Take by weighing 430g piperazine and add 215g of drinking water, fully mix to form material II after stirring, and material II is delivered to the preheating module of microchannel reactor for preheating;

[0031] (3) The preheated material I and material II carry out condensation reaction in the reaction module group, wherein: the flow rate of the slurry pump is adjusted so that the flow rate of the material 1 is 30.0g / min, and the flow rate of the slurry pump is adjusted so that the material I...

Embodiment 2

[0033] (1) take by weighing 198g4, the toluene that 7-dichloroquinoline adds 802g, after stirring, fully stir and mix to dissolve clear and form material I, material I is delivered to the preheating module of microchannel reactor and carry out preheating;

[0034] (2) Take by weighing 430g piperazine and add 215g of drinking water, fully mix to form material II after stirring, and material II is delivered to the preheating module of microchannel reactor for preheating;

[0035](3) The preheated material I and material II carry out condensation reaction in the reaction module group, wherein: the flow velocity of the adjustment slurry pump makes the flow velocity of the material I be 38.0g / min, and the flow velocity of the adjustment slurry pump makes the material I The flow rate of the flow rate is 54.5g / min, the condensation reaction temperature is 109 ℃, the mol ratio of dichloroquinoline and piperazine is 1: 5, and the total residence time of reaction in the reaction module g...

Embodiment 3～9

[0036] Embodiment 3~9: Based on embodiment 1, change the temperature of reaction, other conditions are unchanged, the result that obtains is as follows table.

[0037]

[0038]

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Abstract

The invention discloses a method for synthesizing a piperaquine intermediate by means of a microchannel reactor, and belongs to the technical field of synthesis of antimalarial medicines. The method comprises the steps of dissolving piperaquine in an appropriate amount of water as a material I, dissolving 4,7-dichloroquinoline in an organic solvent as a material, and transporting the material I toa preheating module of the microchannel reactor for preheating; and transporting the preheated material I to a reaction module set of the microchannel reactor, meanwhile, directly transporting the material into the reaction module set of the microchannel reactor, making the material I and the material subjected to condensation reaction, collecting reaction liquid which flows out of an outlet of the microchannel reactor, and obtaining 7-chloro-4-piperazinoquinoline after conducting post-treatment on the reaction liquid. By means of the synthesis method, reaction time can be effectively shortened, so that acid non-soluble substance impurities are greatly reduced.

Description

technical field [0001] The invention belongs to the technical field of medicine and chemical industry, and in particular relates to the synthesis of 7-chloro-4-(1-piperazinyl)quinoline, an intermediate of piperaquine phosphate for treating antimalarial. Background technique [0002] What the present invention relates to is the intermediate of antimalarial piperaquine phosphate (Piperaquine Phosphate), chemical name is 7-chloro-4-(1-piperazinyl) quinoline, CAS number is 837-52-5, chemical The structural formula is as follows: [0003] [0004] Malaria is a serious, sometimes fatal disease caused by a parasite, usually a certain type of mosquito that feeds on humans. People with malaria are usually weak, with high fever, shivering and flu-like illness. Although malaria can be a deadly disease, the illness and death it causes is usually preventable and treatable. According to the latest statistics released by the World Health Organization on April 25, 2008, more than 500 ...

Claims

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Application Information

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IPC IPC(8): C07D215/42
CPCC07D215/42
Inventor 聂光辉蔡中文樊洋杨忠鑫杨继斌张朝东
Owner CHONGQING KANGLE PHARMA
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