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Preparation method for 8-amino-5-methylquinoline

A technology of methylquinoline and amino, applied in the field of preparation of 8-amino-5-methylquinoline, which can solve the problems of long reaction time, high cost and high risk

Inactive Publication Date: 2014-06-25
QINGDAO VLAND BIOTECH INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] For the preparation method of 8-amino-5-methylquinoline, the synthesis methods reported in previous literature mostly use palladium carbon as catalyst for hydrogenation reaction, which requires equipment High, dangerous, long reaction time, high cost and other defects affect the application of 8-amino-5-methylquinoline

Method used

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Examples

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Effect test

preparation example Construction

[0005] The preparation method of the 8-amino-5-methyl pyrine in the present invention is as follows:

[0006] 1. At room temperature, SNCL 2 · 2H 2 O is added to the ethyl acetate solution of 8-nitro-5-methyllyrine, stir 2-3 h;

[0007] 2. Use 10%sodium hydroxide solution to strong alkali;

[0008] 3. Sub-liquid, extract 2-3 times with ethyl acetate, combine organic phase, wash 2-3 times with saturated saline, dry sodium sulfate, filter, steam the dry solvent with a rotary evaporator;

[0009] 4. Reveals with a methanol water solution to obtain 8-amino-5-methyl pyrine.

[0010] The following is a combination of specific instances to further illustrate the present invention.

Embodiment 1

[0012] At room temperature, SNCL 2 · 2H 2 O (90 g, 4.2 EQ) is added to the 8-nitro-5-methyl acerne (18.0 g, 95.7 mmol) acetate solution of 330 ml and stir for 2-3 h.Use 10%sodium hydroxide solution to strong alkali, separate liquid, extract 2-3 times with ethyl acetate, combine organic phase, wash 2-3 times with saturated saline, dry sodium sulfate, filtrate, evaporate with rotation, evaporate with rotationThe instrument steamed dry solvents, the methanol solution was crystal, and the income yield was 100%.

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Abstract

The invention discloses a preparation method for 8-amino-5-methylquinoline. 8-nitro-5-methylquinoline is taken as a raw material, stannous chloride is taken as a reducing agent, a reaction is performed at room temperature, and alkalization, extraction and recrystalization are performed for obtaining 8-amino-5-methylquinoline. In the preparation method, stannous chloride is employed for replacing conventional palladium / carbon for reduction, so that requirements of the reaction on equipment is reduced, reaction dangerousness, reaction time and cost are reduced, but yield is not reduced, and the preparation method has good economic benefit.

Description

Technical field [0001] The present invention involves a preparation method of 8-amino-5-methyl pyrine. Background technique [0002] 8-amino-5-methyl pyrine is an important chemical product and is an important synthetic raw material and intermediate in the field of chemical drugs. [0003] The preparation method of 8-amino-5-methyl pyrine, the synthesis method reported in the past mostly uses carbon carbon as a catalyst to perform hydrogenation reactions.The application of 8-amino-5-methyl pyrine. Invention content [0004] The purpose of the present invention is to provide a preparation method of 8-amino-5-methyl pyrine. This method improves reagents and reduction methods for reactive reagents, and replace the reducing hydrogen carbon dedaming to restore the chloride.The improved preparation method greatly reduces the requirements of the reaction, the risk of reaction, the time and cost of the reaction, the time and cost of the reaction, and the income has not been reduced, and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D215/40
CPCC07D215/40
Inventor 孙伟之孙亚磊毕立学
Owner QINGDAO VLAND BIOTECH INC
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