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Method for preparing 6-aminopurine

A technology of aminopurine and acetylpurine, which is applied in the field of preparation of 6-aminopurine, can solve the problems of few sources of hypoxanthine, no way to achieve large-scale application, and no large-scale source, and achieve high product purity and reaction The effect of mild conditions and simple process methods

Inactive Publication Date: 2012-11-14
JIANGSU QIHE CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Hypoxanthine is chlorinated by phosphorus oxychloride in the presence of tertiary amines to obtain 6-chloropurine, and then adenine can also be obtained by ammoniation (J Am Chem Soc., 1954, 76:6073; J Am Chem Soc., 1982, 104: 3349; J Am Chem Soc., 2007, 129: 7055; J Am Chem Soc., 1990, 112: 8174; Eur J Org Chem,2002,14:2356), but less sources of hypoxanthine , this route has no way to achieve large-scale application
Wang Kai and others synthesized 6-aminopurine (CN102127081) using 4,6-dichloro-5-nitropyrimidine as a raw material, but there is no large-scale source of 4,6-dichloro-5-nitropyrimidine in industry

Method used

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  • Method for preparing 6-aminopurine

Examples

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Effect test

Embodiment 1

[0010] In a 1000ml three-neck flask with a stirring and reflux device, add 177 grams of 6-amino-7-acetylpurine and 400 grams of 10% sodium hydroxide aqueous solution, and heat at 80°C for 2 hours; then add 5 grams of activated carbon and keep warm Decolorize for 1 hour, filter the solution after decolorization, neutralize the filtrate to pH 7 with 10% by mass hydrochloric acid, cool the solution to 0°C; filter again, and dry the filter cake at 50°C for 10 hours to obtain 128 grams of 6-amino Purine, yield 94.8%.

Embodiment 2

[0012] In a 1000ml three-neck flask with a stirring and reflux device, add 177 grams of 6-amino-7-acetylpurine and 560 grams of 30% potassium hydroxide aqueous solution, and heat at 100°C for 6 hours; then add 5 grams of activated carbon and keep warm Decolorize for 3 hours, filter the solution after decolorization, neutralize the filtrate to pH 8 with 30% hydrochloric acid by mass percentage, cool the solution to 10°C; filter again, and dry the filter cake at 100°C for 5 hours to obtain 115 grams of 6-amino Purine, the yield was 85.2%.

Embodiment 3

[0014] In a 1000ml three-necked flask with a stirring and reflux device, add 177 grams of 6-amino-7-acetylpurine and 1000 grams of 20% sodium carbonate aqueous solution, and heat at 90°C for 6 hours; then add 5 grams of activated carbon and keep warm for 2 After decolorization, the solution was filtered after decolorization, and the filtrate was neutralized to pH 7 with 30% by mass percentage of hydrochloric acid, and the solution was cooled to 0°C; then filtered, and the filter cake was dried at 100°C for 5 hours to obtain 130 grams of 6-aminopurine , The yield is 96.3%.

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Abstract

The invention discloses a method for preparing 6-aminopurine. The method is characterized by comprising the following steps: feeding 6-amino-7-acetylpurine and alkali according to a molar ratio of 1:(1-3), reacting the mixture at a temperature of 80 DEG C to 100 DEG C for 2 to 6 hours, adding activated carbon, keeping the temperature for 1 to 3 hours, performing de-coloration, filtering the solution after de-coloration, neutralizing the filtered solution by hydrochloric acid with a mass percent being 10% to 50% until the pH reaches 7 to 8, cooling the solution to a temperature of 0 DEG C to 10 DEG C, performing filtering again, drying a filter cake at a temperature of 50 DE GC to 100 DEG C for 5 to 10 hours, and obtaining the 6-aminopurine. The method for preparing 6-aminopurine has the advantages that the technique is simple, reaction conditions are mild, the product purity is high, and the method is suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of a compound, in particular to a preparation method of 6-aminopurine. Background technique [0002] 6-Aminopurine, Chinese alias: adenine; English name: Adenine English alias: 6-Aminopurine; Vitamin B4, has phytokinin effect, and its tablet or injection can be used for granulocytopenia, etc. It can also be used in tissue culture, biochemical reagents and synthetic drugs such as vitamin B4, purine drugs and other raw materials. Also used in biochemical and pharmaceutical analysis. According to the difference of starting materials, the synthetic method of 6-aminopurine can be summarized into following four kinds. Shanghai Twelfth Pharmaceutical Factory (Chinese Journal of Pharmaceutical Industry, 1972, 5:17) used diethyl malonate as the initial raw material, and underwent six steps of cyclization, nitration, chlorination, ammonification, cyclization, and salt formation. Obtained, this method reaction ste...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D473/34
Inventor 李显龙蒋成君邢小蓬黄建军
Owner JIANGSU QIHE CHEM