Method for synthesizing 2-amino-5-chlorobenzophenone by microchannel reactor

A technology of microchannel reactor and chlorobenzophenone, which is applied in chemical instruments and methods, chemical/physical/physical chemical reactors, preparation of organic compounds, etc., can solve the problems of long reaction time, low times of catalyst recovery and mechanical application, etc. Violent explosion and other problems, to achieve the effect of improving recycling efficiency, increasing intrinsic reaction speed, and reducing degradation impurities

Active Publication Date: 2018-04-20
HEILONGJIANG XINCHUANG BIOLOGICAL TECH DEV CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the problems of low yield, poor purity, danger of violent explosion, long reaction time at high temperature, degradation of catalyst, and low frequency of catalyst recycling in the synthes

Method used

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  • Method for synthesizing 2-amino-5-chlorobenzophenone by microchannel reactor
  • Method for synthesizing 2-amino-5-chlorobenzophenone by microchannel reactor
  • Method for synthesizing 2-amino-5-chlorobenzophenone by microchannel reactor

Examples

Experimental program
Comparison scheme
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Example Embodiment

[0034] Example 1. A method for synthesizing 2-amino-5 chlorobenzophenone in a microchannel reactor.

[0035] 1) Weigh 150g of the raw material 5-chloro-3-phenyl-2,1-benzisoxazole, add 1.2L of anhydrous methanol and 1.2L of tetrahydrofuran, stir to dissolve and add 5g of Pt with a Pt content of 5%. C catalyst is fully stirred and mixed to form material I. Adjust the flow rate of the slurry pump so that the flow rate of material I is 45.0 g / min and enter the preheating module of the microreactor.

[0036] 2) Adjust H 2 The flow rate of the gas flow meter is 400ml / min, which directly enters the reaction module group without preheating to undergo catalytic hydrogenation reaction with material I, such as figure 2 As shown, the molar ratio of 5-chloro-3-phenyl-2,1-benzisoxazole to hydrogen is 1:1.2, the reaction temperature is 50°C, the residence time of the reaction is 30s, and the reaction pressure is 1.5Mpa; Then enter the cooling module, the temperature of the cooling module is 20°...

Example Embodiment

[0037] Example 2. A method for synthesizing 2-amino-5 chlorobenzophenone in a microchannel reactor.

[0038] 1) Weigh 180g of the raw material 5-chloro-3-phenyl-2,1-benzisoxazole, add 1.5L of absolute ethanol and 1.5L of ethyl acetate, stir to dissolve, add 9g of Pd content of 10% The Pd / C catalyst is fully stirred and mixed to form material I. Adjust the flow rate of the slurry pump so that the flow rate of material I is 42.0 g / min, and enter the preheating module of the microreactor.

[0039] 2) Adjust H 2 The flow rate of the gas flow meter is 350ml / min, which directly enters the reaction module group without preheating to undergo catalytic hydrogenation reaction with material I, such as figure 2 As shown, the molar ratio of 5-chloro-3-phenyl-2,1-benzisoxazole to hydrogen is 1:1.1, the reaction temperature is 80°C, the residence time of the reaction is 32s, and the reaction pressure is 1.2Mpa; Then enter the cooling module, the temperature of the cooling module is 20°C, collec...

Example Embodiment

[0040] Example 3. A method for synthesizing 2-amino-5 chlorobenzophenone in a microchannel reactor.

[0041] 1) Weigh 200g of the raw material 5-chloro-3-phenyl-2,1-benzisoxazole, add 1.5L of anhydrous methanol and 1.5L of tetrahydrofuran, stir to dissolve and add 20g of Pd with a Pd content of 3%. Catalyst C is fully stirred and mixed to form material I. Adjust the flow rate of the slurry pump so that the flow rate of material I is 40.0 g / min, and enter the preheating module of the microreactor.

[0042] 2) Adjust H 2 The flow rate of the gas flow meter is 500ml / min, which directly enters the reaction module group without preheating to undergo catalytic hydrogenation reaction with material I, such as figure 2 As shown, the molar ratio of 5-chloro-3-phenyl-2,1-benzisoxazole to hydrogen is 1:1.5, the reaction temperature is 90°C, the residence time of the reaction is 40s, and the reaction pressure is 0.6Mpa; Then enter the cooling module, the temperature of the cooling module is 2...

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Abstract

The invention discloses a method for synthesizing 2-amino-5-chlorobenzophenone by a microchannel reactor, belongs to the field of synthesis of psychoactive drugs in organic synthesis, and solves the problems of low yield, poor purity, high risk of violent explosion, degradation caused by high reaction time under high temperature and high pressure conditions, low frequency of catalyst recycling andreuse and the like during the synthesis of a traditional catalytic hydrogenation reactor. The method for synthesizing the 2-amino-5-chlorobenzophenone in the microchannel reactor specifically includes the following steps: 1). adding hydrogenation reaction precursor 5-chloro-3-phenyl-2,1-benzisoxazole into an organic solvent, and then adding an activated-carbon-loaded noble metal catalyst to obtain a mixture as a material I to enter a preheating module of the microreactor; and 2). after preheating of the material I, injecting the material I and material II hydrogen into a reaction module groupof the microreactor for reaction, collecting a reaction solution flowing out from a cooling module, and treating to obtain the 2-amino-5-chlorobenzophenone. The method is suitable for the large-scaleproduction of the 2-amino-5-chlorobenzophenone.

Description

technical field [0001] The invention belongs to the field of synthesis of psychotropic drugs in organic synthesis, and in particular relates to a synthesis method of 2-amino-5-chlorobenzophenone. Background technique [0002] 2-Amino-5-chlorobenzophenone is an important intermediate for the synthesis of diazepam, chlordiazepoxide, oxazepam and other benzodiazepine hypnotic and sedative drugs. Diazepine hypnotic and sedative drugs are mainly used in Treatment of anxiety and various functional neurosis, insomnia, especially anxiety insomnia treatment is excellent. At the same time, 2-amino-5-chlorobenzophenone derivatives are widely used in anti-cancer, anti-mitosis, receptor antagonists, anti-osteoporosis, etc., and are also important raw materials for the synthesis of quinoline by the Friedlander method. As a very commonly used and important intermediate in the field of medicine and chemical industry, the advantages and disadvantages of its synthesis method are of great eco...

Claims

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Application Information

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IPC IPC(8): C07C225/22C07C221/00B01J19/00
CPCB01J19/0093C07C221/00C07C225/22Y02P20/584
Inventor 任吉秋杨昆李海涛
Owner HEILONGJIANG XINCHUANG BIOLOGICAL TECH DEV CO LTD
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