Preparation method of R-7-chloro-1-tetralinylamine

A technology of tetralamine and R-7-, which is applied in the field of synthesis and resolution of chiral amines, to achieve the effects of good product yield, great guidance and application value, and high purity

Inactive Publication Date: 2017-02-08
王际菊
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Through the research literature, it can be found that there is no information about how to use kinetics and dynamic kinetics resolution to prepare R-7-chloro-1,2,3,4-tetrahydronaphthalene-1-amine

Method used

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  • Preparation method of R-7-chloro-1-tetralinylamine

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Embodiment 1

[0006] 1) Preparation of 7-chloro-1,2,3,4-tetrahydronaphthalene-1-amine

[0007] In a 1000ml autoclave, add 90g 7-chloro-1-tetralone, 600ml anhydrous ethanol, 12g catalyst SN-600P, seal the reaction kettle, use a vacuum pump to remove the air in the kettle, and then fill with nitrogen to 0.5MPa, and then use The vacuum pump is used for vacuuming; 80g ammonia gas is charged under negative pressure. After the ammonia gas is filled, the autoclave is charged with hydrogen gas to 4MPa and heated to 90°C for reaction. After 9 hours of reaction, it was found that the hydrogen pressure did not drop anymore, and the reaction was stopped. After the temperature of the system drops to room temperature, the reaction solution is filtered and concentrated to obtain crude 7-chloro-1,2,3,4-tetrahydronaphthalene-1-amine. Add the crude product to the dilute hydrochloric acid solution with stirring, let it react to form 7-chloro-1,2,3,4-tetrahydronaphthalene-1-amine salt, and dissolve it in the aqu...

Embodiment 2

[0013] 1) Preparation of 7-chloro-1,2,3,4-tetrahydronaphthalene-1-amine

[0014] In a 1000ml autoclave, add 90g 7-chloro-1-tetralone, 600ml anhydrous ethanol and 10g catalyst SN-600P, seal the reaction kettle, use a vacuum pump to remove the air in the kettle, then fill with nitrogen to 0.5MPa, and then use The vacuum pump is used for vacuuming; under negative pressure, 51g of ammonia is filled. After the ammonia is filled, the autoclave is filled with hydrogen to 4MPa, and the temperature is raised to 80°C for reaction. After reacting for 10 hours, it was found that the hydrogen pressure no longer dropped, and the reaction was stopped. After the temperature of the system drops to room temperature, the reaction solution is filtered and concentrated to obtain crude 7-chloro-1,2,3,4-tetrahydronaphthalene-1-amine. Add the crude product to the dilute hydrochloric acid solution with stirring, let it react to form 7-chloro-1,2,3,4-tetrahydronaphthalene-1-amine salt, and dissolve it in...

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Abstract

The invention discloses a preparation method of R-7-chloro-1-tetralinylamine. The method comprises the following steps: carrying out reduction ammonification reaction on the raw material 7-chloro-1-tetralone to obtain 7-chloro-1,2,3,4-tetrahydronaphthyl-1-amine, and carrying out dynamic kinetic resolution on the 7-chloro-1,2,3,4-tetrahydronaphthyl-1-amine by using the combination of lipase and a racemization catalyst to obtain the R-7-chloro-1,2,3,4-tetrahydronaphthyl-1-amine. The method is simple to operate, and has the characteristics of wide raw material sources, favorable product yield, high optical purity of the resolution product and the like.

Description

Technical field [0001] The present invention relates to a method for synthesis and resolution of chiral amines, in particular to a dynamic power for synthesizing 7-chloro-1,2,3,4-tetrahydronaphthalene-1-amine by chemical method and then by enzyme catalysis Learn how to split. Background technique [0002] 7-chloro-1,2,3,4-tetrahydronaphthalene-1-amine is used as a chiral intermediate. In the existing related research, there are few reports on how to prepare and resolve 7-chloro-1,2,3,4-tetrahydronaphthalene-1-amine. It can be found through the research literature that there is no information on how to use kinetics and dynamic kinetic resolution to prepare R-7-chloro-1,2,3,4-tetrahydronaphthalene-1-amine. Summary of the invention [0003] The present invention aims to provide a method for synthesizing 7-chloro-1,2,3,4-tetrahydronaphthalene-1-amine and kinetic resolution to obtain 7-chloro-1,2,3,4 -Tetrahydronaphthalene-1-amine. In order to achieve this goal, the specific operat...

Claims

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Application Information

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IPC IPC(8): C12P41/00C12P13/02C07C209/28C07C211/42
CPCC07C209/28C12P13/02C12P41/007C07C211/42
Inventor 王际菊
Owner 王际菊
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