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
View PDF2 Cites 4 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 int

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • 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

Examples

Experimental program
Comparison scheme
Effect test

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 ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C07D471/04
CPCC07D471/04
Inventor 任吉秋杨昆李海涛
Owner HEILONGJIANG XINCHUANG BIOLOGICAL TECH DEV CO LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap