Preparation method for 8-amino-7-methylquinoline

A methylquinoline and amino technology, which is applied in the field of preparation of 8-amino-7-methylquinoline, can solve the problems of high equipment requirements, high cost, affecting the application of 8-amino-7-methylquinoline and the like

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-7-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-7-methylquinoline

Method used

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Examples

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Effect test

preparation example Construction

[0005] The preparation method step of 8-amino-7-methylquinoline among the present invention is as follows:

[0006] 1. At room temperature, the SnCl 2 2H 2 O was added to the ethyl acetate solution of 8-nitro-7-methylquinoline in portions, and stirred for 2-3 h;

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

[0008] 3. Separate the liquid, extract 2-3 times with ethyl acetate, combine the organic phases, wash 2-3 times with saturated brine, dry over anhydrous sodium sulfate, filter, and evaporate the solvent to dryness with a rotary evaporator;

[0009] 4. Recrystallize with aqueous methanol to obtain 8-amino-7-methylquinoline.

[0010] The present invention is further illustrated below in conjunction with specific examples.

Embodiment 1

[0012] At room temperature, the SnCl 2 2H 2 O (90 g, 4.2 eq) was added in portions to 330 mL of a solution of 8-nitro-7-methylquinoline (18.0 g, 95.7 mmol) in ethyl acetate, and stirred for 2-3 h. Use 10% sodium hydroxide solution to adjust to strong alkalinity, separate the layers, extract 2-3 times with ethyl acetate, combine the organic phases, wash 2-3 times with saturated brine, dry over anhydrous sodium sulfate, filter, and use rotary evaporation The solvent was evaporated to dryness, recrystallized from methanol aqueous solution, and the yield was 100%.

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Abstract

The invention discloses a preparation method for 8-amino-7-methylquinoline. 8-nitro-7-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-7-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 invention relates to a preparation method of 8-amino-7-methylquinoline. Background technique [0002] 8-Amino-7-methylquinoline is an important chemical product and an important synthetic raw material and intermediate in the field of chemical medicine. [0003] The preparation method of 8-amino-7-methylquinoline, the synthesis method reported in the past mostly uses palladium carbon as a catalyst for hydrogenation reaction, which has defects such as high equipment requirements, high risk, long reaction time and high cost, which affect The application of 8-amino-7-methylquinoline. Contents of the invention [0004] The object of the present invention is to provide a kind of preparation method of 8-amino-7-methylquinoline, this method has been improved to the reagent of reaction and reduction method, and palladium-carbon hydrogenation reduction is replaced by stannous chloride reduction. The improved preparation method greatly reduces the req...

Claims

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Application Information

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IPC IPC(8): C07D215/40
CPCC07D215/40
Inventor 孙伟之姚德勇侯青青
Owner QINGDAO VLAND BIOTECH INC
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