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Adenine synthesis technology

A synthesis process and adenine technology, applied in the field of adenine synthesis technology, can solve the problems of large amount of three wastes treatment, many reaction steps, low yield and the like, and achieve the effects of improving production efficiency, reducing processing cost and simple process

Inactive Publication Date: 2014-07-16
XINXIANG RUICHENG TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition to being prepared by the total synthesis of diethyl malonate, the current industrial production of adenine in domestic manufacturers is based on hypoxanthine as a starting material, which is mixed with phosphorus oxychloride and N,N-dimethylaniline. Chlorination, hydrolysis, pressurized ammoniation, refining and other reaction synthesis, many reaction steps, low yield, large amount of three wastes treatment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0008] First, add the measured 110 parts by weight of acetic anhydride into the dry reaction kettle, start stirring at the same time, slowly add 38 parts by weight of adenosine, heat it to 110°C with the jacket, and use the remaining temperature of the jacket to dissolve the adenosine. After clearing, add 2.5 parts by weight of boric acid and react at 110°C. After 1.5 hours, the reaction solution gradually becomes turbid. Continue to heat at 110°C for 10 hours and then cool down overnight; (2) Separate the above reaction solution by suction filtration, and the filter cake is Acetyl adenine, dried for later use; (3) The mother liquor in step (2) is concentrated by negative pressure to dry the mixed solution of acetic acid and acetic anhydride. After dividing the water, pump the syrup into the kettle, wash with water, cool down to 20°C to crystallize, and filter to obtain the crude tetraacetyl ribose; (4) The crude tetraacetyl ribose in step 3 is dissolved by 100 parts by weight ...

Embodiment 2

[0010] First, add the measured 115 parts by weight of acetic anhydride into the dry reaction kettle, start stirring at the same time, slowly put in 39 parts by weight of adenosine, heat it to 110°C with the jacket, and use the remaining temperature of the jacket to dissolve the adenosine. After clearing, add 3 parts by weight of boric acid, and keep it warm at 115°C for reaction. After 2 hours, the reaction solution gradually becomes turbid. Continue to keep warm at 115°C for 10 hours and then cool down overnight; (2) Separate the above reaction solution by suction filtration, and the filter cake is Acetyl adenine, dried for later use; (3) The mother liquor in step (2) is concentrated by negative pressure to dry the mixture of acetic acid and acetic anhydride, and the obtained syrup is added to the pre-prepared reaction kettle with a measured weight of 105 After the water is divided, the syrup is pumped into the kettle, washed with water, cooled to 20°C to crystallize, and filt...

Embodiment 3

[0012] First, add 120 parts by weight of acetic anhydride measured into the dry reaction kettle, start stirring at the same time, slowly add 40 parts by weight of adenosine, heat to 110°C with the jacket, and use the remaining temperature of the jacket to dissolve the adenosine. After clearing, add 3.5 parts by weight of boric acid, and keep warm at 113°C for reaction. After 2.5 hours, the reaction solution gradually becomes cloudy. Continue to keep warm at 112°C for 10 hours and then cool down overnight; (2) The above reaction solution is separated by suction filtration, and the filter cake is Acetyl adenine, dried for later use; (3) The mother liquor in step (2) is concentrated by negative pressure to dry the mixed solution of acetic acid and acetic anhydride. After dividing the water, pump the syrup into the kettle, wash with water, cool down to 20°C to crystallize, and filter to obtain the crude tetraacetyl ribose; (4) The crude tetraacetyl ribose in step 3 is dissolved by ...

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PUM

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Abstract

The invention discloses an adenine synthesis technology. The adenine synthesis technology comprises the following steps: acetylating adenosine serving as a substrate by using acetic anhydride so as to obtain acetylated adenine and tetraacetylribose, carrying out alkaline hydrolysis on the acetylated adenine, and neutralizing the acetylated adenine so as to obtain adenine. The adenine synthesis technology is simple, very beneficial to the large-scale production of the adenine and capable of greatly reducing the processing cost of the adenine and improving the production efficiency of the adenine.

Description

Technical field: [0001] The invention relates to the manufacture of adenine, in particular to an adenine synthesis process. Background technique: [0002] Adenine, whose chemical name is 6-aminopurine, is the main raw material for the synthesis of vitamin B4. Every year, hundreds of tons of adenine are exported to the international market for the preparation of purine derivatives and other drugs. In addition to being prepared by the total synthesis of diethyl malonate, the current industrial production of adenine in domestic manufacturers is based on hypoxanthine as a starting material, which is mixed with phosphorus oxychloride and N,N-dimethylaniline. Chlorination, hydrolysis, pressurized ammoniation, refining and other reaction synthesis, many reaction steps, low yield, large amount of three wastes treatment. Invention content: [0003] The purpose of the present invention is to provide an adenine synthesis process with simple process and favorable for large-sc...

Claims

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Application Information

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IPC IPC(8): C07D473/34
CPCC07D473/34
Inventor 张成立
Owner XINXIANG RUICHENG TECH DEV
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