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Synthesizing method of 3-chloro-7-azaindole

A technique for the synthesis of azaindole and its synthesis method, which is applied in the field of synthesis of 3-chloro-7-azaindole, and can solve the problems of N-chlorosuccinimide with high toxicity, unfriendly environment and complex process, etc. , to achieve the effect of easy control, high product purity and low operation difficulty

Inactive Publication Date: 2017-10-10
BTC PHARMA TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] 3-Chloro-7-azaindole is widely used in pharmaceutical intermediates. At present, N-chlorosuccinimide is generally used as a chlorination reagent for production. N-chlorosuccinimide is highly toxic and cumbersome to handle. , not friendly to the environment, high cost, complicated process, urgently need safe and environmentally friendly, low-cost and simple process, scientific production, increase production, but the current technology is difficult

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] The method for synthesizing 3-chloro-7-azaindole of the present invention,

[0015] Put 450ml acetone and 90g 7-azaindole into a 1000ml four-neck flask;

[0016] Start stirring and use low temperature cooling cycle to cool down to 15℃;

[0017] Add 59.4g of strong chlorinate in batches, 5.4g in 11 batches, and control the temperature below 20°C. After the addition, stir at 20°C for 1 hour. HPLC detects that the reaction of the raw materials is complete;

[0018] Add 450ml water dropwise to the raw materials, filter with filter cake, and rinse the filter cake with 90ml water respectively. After drying, 107 g of light yellow solid was obtained, the content was 98.2%, and the yield was 92%.

Embodiment 2

[0020] The method for synthesizing 3-chloro-7-azaindole of the present invention,

[0021] Put 550ml acetone and 110g 7-azaindole into a 1000ml four-neck flask;

[0022] Start stirring and use low temperature cooling cycle to cool down to 15℃;

[0023] Add 72.6g of strong chlorinate in batches, 6.6g each in 11 batches, and control the temperature below 20°C. After the addition, stir at 20°C for 1 hour. HPLC detects that the reaction of the raw materials is complete;

[0024] Add 550ml water dropwise to the raw materials, filter with filter cake, and rinse the filter cake with 110ml water respectively. After drying, 131 g of light yellow solid was obtained, the content was 98.1%, and the yield was 92.1%.

Embodiment 3

[0026] The method for synthesizing 3-chloro-7-azaindole of the present invention,

[0027] Add 600ml acetone and 120g 7-azaindole into a 1000ml four-neck flask;

[0028] Start stirring and use low temperature cooling cycle to cool down to 15℃;

[0029] 72.9g strong chlorinate was added in batches, 7.2g each in 11 batches, and the temperature was controlled below 20°C. After the addition was completed, stirred at 20°C for 1 hour, and the reaction of the raw materials was detected by HPLC.

[0030] Add 600ml water dropwise to the raw materials, filter with filter cake, and rinse the filter cake with 120ml water respectively. After drying, 145 g of light yellow solid was obtained, the content was 98.8%, and the yield was 93.4%.

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PUM

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Abstract

The invention discloses a synthesizing method of 3-chloro-7-azaindole. The synthesizing method comprises the following steps of by using 7-azaindole as a raw material, reacting with trichloroisocyanuric acid to synthesize. The synthesizing method has the advantages that the trichloroisocyanuric acid is used as a chlorinating reagent, the pollution to environment is smaller, the cost is low, the difficulty in operation is low, the output is conveniently increased, the control is easy, and the product purity is high.

Description

Technical field [0001] The invention relates to a method for synthesizing 3-chloro-7-azaindole. Background technique [0002] 3-Chloro-7-azaindole is widely used in pharmaceutical intermediates. At present, N-chlorosuccinimide is generally used as a chlorinating reagent for production. N-chlorosuccinimide is more toxic and cumbersome to handle , It is not friendly to the environment, the cost is high, and the process is complex. There is an urgent need for safe and environmentally friendly, low-cost and simple processes to carry out scientific production and increase production. However, the current technology is difficult. [0003] Therefore, it is necessary to provide a new technical solution to solve the above-mentioned problems. Summary of the invention [0004] The technical problem to be solved by the invention is to provide a method for synthesizing 3-chloro-7-azaindole. [0005] A method for synthesizing 3-chloro-7-azaindole, including the following steps: [0006] Put 500ml...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D471/04
CPCC07D471/04
Inventor 陈国庆吴加朋李怀鑫杨少强周广徐本全
Owner BTC PHARMA TECH CO LTD