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Method for utilizing microchannel reactor to synthesize paliperidone midbody

A technology of microchannel reactor and paliperidone, which is applied in the direction of organic chemistry, can solve the problems of low catalyst recycling times, prone to violent explosion, and long reaction time, so as to shorten the process development cycle, short reaction time, Small liquid retention effect

Active Publication Date: 2018-05-08
HEILONGJIANG XINCHUANG BIOLOGICAL TECH DEV CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0015] In order to solve the problems of low yield, poor purity, danger of severe explosion, long reaction time at high temperature, degradation of catalyst, and low number of times of catalyst recycling in traditional synthesis reactions, the present invention provides an intrinsically safe and environmentally friendly 3- Catalytic hydrogenation synthesis technology of (2-chloroethyl)-6,7,8,9-tetrahydro-9-hydroxy-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one , especially a method for synthesizing paliperidone intermediates using a microchannel reactor

Method used

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  • Method for utilizing microchannel reactor to synthesize paliperidone midbody
  • Method for utilizing microchannel reactor to synthesize paliperidone midbody
  • Method for utilizing microchannel reactor to synthesize paliperidone midbody

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Embodiment 1

[0046] Present embodiment provides a kind of method utilizing microchannel reactor to synthesize paliperidone intermediate, such as figure 1 and figure 2 As shown, the microchannel reactor includes a preheating module, a reaction module group and a cooling module, wherein: the preheating module is connected in series with the reaction module group, the reaction module group is connected in series with the cooling module, and the reaction module group includes a unit reaction module or It is formed by combining more than two unit reaction modules in series; the method for synthesizing the paliperidone intermediate comprises the following steps:

[0047] 1) Weigh 200 g of paliperidone hydrogenation precursor 3-(2-chloroethyl)-2-methyl-9-hydroxy-4H-pyrido[1,2-A]pyrimidin-4-one, add 4L of absolute ethanol, 200g of concentrated hydrochloric acid, after stirring evenly, add 5g of 10% Pd / C, fully stir and mix to form material I;

[0048] 2) The material I and hydrogen after step ...

Embodiment 2

[0050] Present embodiment provides a kind of method utilizing microchannel reactor to synthesize paliperidone intermediate, such as figure 1 and figure 2 As shown, the microchannel reactor includes a preheating module, a reaction module group and a cooling module, wherein: the preheating module is connected in series with the reaction module group, the reaction module group is connected in series with the cooling module, and the reaction module group includes a unit reaction module or It is formed by combining more than two unit reaction modules in series; the method for synthesizing the paliperidone intermediate comprises the following steps:

[0051] 1) Weigh 200 g of paliperidone hydrogenation precursor 3-(2-chloroethyl)-2-methyl-9-hydroxy-4H-pyrido[1,2-A]pyrimidin-4-one, add 4L of anhydrous methanol, 150g of concentrated hydrochloric acid, after stirring evenly, add 5g of 5% Pt / C, fully stir and mix to form material I;

[0052] 2) The material I and hydrogen after step...

Embodiment 3

[0054] Present embodiment provides a kind of method utilizing microchannel reactor to synthesize paliperidone intermediate, such as figure 1 and figure 2 As shown, the microchannel reactor includes a preheating module, a reaction module group and a cooling module, wherein: the preheating module is connected in series with the reaction module group, the reaction module group is connected in series with the cooling module, and the reaction module group includes a unit reaction module or It is formed by combining more than two unit reaction modules in series; the method for synthesizing the paliperidone intermediate comprises the following steps:

[0055] 1) Weigh 300g of paliperidone hydrogenation precursor 3-(2-chloroethyl)-2-methyl-9-hydroxyl-4H-pyrido[1,2-A]pyrimidin-4-one, add 6L of absolute ethanol, 200g of concentrated hydrochloric acid, after stirring evenly, add 5g of 10% Rh / C, fully stir and mix to form material I;

[0056] 2) The material I and hydrogen after step ...

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Abstract

The invention discloses a method for utilizing a microchannel reactor to synthesize a paliperidone midbody, and belongs to the technical field of psychotropic medicine synthesis in organic synthesis.By means of the method, a paliperidone hydrogen-adding reaction precursor 3-(2-chloroethyl)-2-methyl-9-hydroxyl-4H-pyridino-[1,2-A]pyrimidine-4-ketone is added into an organic solvent, after a catalyst of activated-carbon-loaded precious metal is added, the mixture is used as a first material, and the first material is delivered into a preheating module of the microchannel reactor to be preheated;the preheated first material and hydrogen are delivered to a reaction module of the microchannel reactor separately to be reacted, reaction liquid flowing out of an outlet of the microchannel reactoris collected, and the paliperidone midbody is obtained through aftertreatment. By means of the synthesis method, the reaction time can be effectively shortened, the potential safety hazard of a hydrogen leakage combustion explosion is greatly lowered, and the method is applicable to synthesizing the paliperidone midbody.

Description

technical field [0001] The invention relates to a method for synthesizing a paliperidone intermediate by using a microchannel reactor, and belongs to the technical field of synthesis of psychotropic drugs in organic synthesis. Background technique [0002] The Chinese name of paliperidone is: 3-[2-[4-(6-fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]-ethyl]-6 ,7,8,9-tetrahydro-9-hydroxy-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one, molecular formula: C 23 h 27 FN 4 o 3 , the chemical structure is as follows [0003] [0004] The drug was approved by the US FDA on December 19, 2006 for the acute or maintenance treatment of schizophrenia. Studies have shown that paliperidone can delay the relapse rate of schizophrenia and is used for acute short-term and long-term maintenance treatment of schizophrenia. , relieve symptoms, and long-term use can effectively stabilize the patient's condition. [0005] Compound 3-(2-chloroethyl)-6,7,8,9-tetrahydro-9-hydroxy-2-methyl-4H-pyrido[1...

Claims

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Application Information

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IPC IPC(8): C07D471/04
CPCC07D471/04
Inventor 任吉秋杨昆李海涛
Owner HEILONGJIANG XINCHUANG BIOLOGICAL TECH DEV CO LTD
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