Preparation method of 5-bromine-7-azaindole

A technology of azaindole and bromine, which is applied in the field of preparation of 5-bromo-7-azaindole, can solve the problems of complicated operation, complicated preparation process, complicated process, etc., and achieves low requirements for preparation environment and high preparation efficiency. Simple method and low operation difficulty

Inactive Publication Date: 2019-01-18
ABA CHEM CORP
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the deficiencies of the prior art, the present invention provides a preparation method of 5-bromo-7-azaindole, which has the advantages of low cost and high proportion of 5-bromo-7-azaindole, and solves the problem of traditional The preparation process of the 5-bromo-7-azaindole is complicated, and 2-aminopyridine is used as a raw material through bromination, coupling, and ring closure. Low, users often need to spend a lot of time in the preparation of 5-bromo-7-azaindole, and the purity of the prepared 5-bromo-7-azaindole is low, and the input is not proportional to the harvest

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment one: a kind of preparation method of 5-bromo-7-azaindole, comprises the following steps:

[0020] 1) Prepare 200 mg of 2-aminopyridine, 100 mg of dimethyl sulfoxide, 500 mg of sodium carbonate solution, 100 mg of 7-azaindole, 500 mg of anhydrous sodium sulfate, and 50 mg of N-bromosuccinimide , ethyl acetate 20 mg, bromine 600 mg, alcohol solvent 100 mg and dihydro-7-azaindole-2-sulfonic acid sodium salt 600 mg, users take 2-aminopyridine 200 mg and 7-nitrogen Heat 100 mg of Zaindole to 50 degrees Celsius for use;

[0021] 2) Take out 200 mg of 2-aminopyridine and 100 mg of 7-azaindole heated to 50 degrees Celsius, mix them, stir with a glass rod at a frequency of 150 rpm, and add 100 mg of dimethyl sulfoxide in batches after ten minutes mg and 500 mg of sodium carbonate solution to obtain a mixture 1, pour the mixture 1 into a beaker, heat the mixture 1 to 80-85 degrees Celsius, and stir the mixture 1 clockwise at a frequency of 300 revolutions per minute w...

Embodiment 2

[0029] Embodiment two: a kind of preparation method of 5-bromo-7-azaindole, comprises the following steps:

[0030] 1) Prepare 500 mg of 2-aminopyridine, 150 mg of dimethyl sulfoxide, 800 mg of sodium carbonate solution, 200 mg of 7-azaindole, 700 mg of anhydrous sodium sulfate, and 60 mg of N-bromosuccinimide , ethyl acetate 30 mg, bromine 800 mg, alcohol solvent 300 mg and dihydro-7-azaindole-2-sulfonic acid sodium salt 800 mg, the user takes 2-aminopyridine 500 mg and 7-nitrogen Heat 200 mg of Zaindole to 60 degrees Celsius for use;

[0031] 2) Take out 500 mg of 2-aminopyridine and 200 mg of 7-azaindole heated to 50-60 degrees Celsius, mix them, stir with a glass rod at a frequency of 150 rpm, and add dimethyl methoxide in batches after ten minutes 150 mg of sulfone and 800 mg of sodium carbonate solution to obtain a mixture 1, pour the mixture 1 into a beaker, heat the mixture 1 to 80-85 degrees Celsius, and stir the mixture 1 clockwise with a glass rod at a rate of 300 ...

Embodiment 3

[0039] Embodiment three: a kind of preparation method of 5-bromo-7-azaindole, comprises the following steps:

[0040] 1) Prepare 350 mg of 2-aminopyridine, 125 mg of dimethyl sulfoxide, 650 mg of sodium carbonate solution, 150 mg of 7-azaindole, 600 mg of anhydrous sodium sulfate, and 55 mg of N-bromosuccinimide , ethyl acetate 25 mg, bromine 700 mg, alcohol solvent 200 mg and dihydro-7-azaindole-2-sulfonic acid sodium salt 700 mg, the user takes 2-aminopyridine 350 mg and 7-nitrogen Heat 150 mg of Zaindole to 50-60 degrees Celsius for use;

[0041] 2) Take out 350 mg of 2-aminopyridine and 150 mg of 7-azaindole heated to 50-60 degrees Celsius, mix them, stir with a glass rod at a frequency of 150 revolutions per minute, and add dimethyl methoxide in batches after ten minutes 125 mg of sulfone and 650 mg of sodium carbonate solution to obtain a mixture 1, pour the mixture 1 into a beaker, heat the mixture 1 to 80-85 degrees Celsius, and stir the mixture 1 clockwise with a gla...

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Abstract

The invention relates to the technical field of medicine and discloses a preparation method of 5-bromine-7-azaindole. The preparation method of the 5-bromine-7-azaindole comprises the following steps:preparing 200 to 500 mg of 2-aminopyridine, 100 to 150 mg of dimethylsulfoxide, 500 to 800 g of sodium carbonate solution, 100 to 200 mg of 7-azaindole, 500 to 700 mg of anhydrous sodium sulfate, 50to 60 mg of N-bromo-succinimide, 20 to 30 mg of ethyl acetate, 600 to 800 mg of bromine, 100 to 300 mg of alcohol solvent and 600 to 800 mg of dihydro-7-azaindole-2-sodium sulfonate, taking 200 to 500mg of 2-aminopyridine and 100 to 200 mg of 7-azaindole by a user, heating for future use, and taking out the heated 200 to 500 mg of 2-aminopyridine and 100 to 200 mg of 7-azaindole. According to thepreparation method of the 5-bromine-7-azaindole, the 5-bromine-7-azaindole crude product can be prepared by four steps; the preparation method is simple, low in operation difficulty and low requirement on the preparation environment; the user invests small cost to gain great harvest, the trouble of the user is avoided and preparation of the user is facilitated.

Description

technical field [0001] The invention relates to the technical field of medicine, in particular to a preparation method of 5-bromo-7-azaindole. Background technique [0002] Chemicals refer to pure substances and mixtures of various elements, whether natural or man-made. According to the American Chemical Abstracts, there are as many as 7 million chemicals in the world, of which 100,000 have been listed as commodities. There are more than 70,000 kinds of chemicals that are frequently used, and more than 1,000 kinds of chemicals appear in the world every year. According to the degree and type of danger of chemicals, the three words "Danger", "Warning" and "Caution" are respectively used Hazard warning. [0003] The traditional preparation process of 5-bromo-7-azaindole is complicated. It uses 2-aminopyridine as raw material, and it is formed through bromination, coupling and ring closure. Low, users often need to spend a lot of time when preparing 5-bromo-7-azaindole, and th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D471/04
CPCC07D471/04
Inventor 徐军蒋信义张敏华周宇徐萌
Owner ABA CHEM CORP
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