Preparation method of N2,9-diacetylguanine

A technology of diacetylguanine and guanine, which is applied in the chemical field, can solve the problem that the reaction conversion rate only reaches 60%, and achieve the effects of good particle size, reduced energy consumption, and reduced dosage

Active Publication Date: 2016-12-21
STAR LAKE BIOSCI CO INC ZHAOQING GUANGDONG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the advantages of low toxicity and simple operation, but the reaction takes 18 to 23 hours, the temperature requires 120°C, and the reaction conversion rate only reaches 60%.

Method used

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  • Preparation method of N2,9-diacetylguanine
  • Preparation method of N2,9-diacetylguanine
  • Preparation method of N2,9-diacetylguanine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] In a 500ml three-necked flask, add 240g of pyridine, 20g of guanine, and 1g of DMAP (4-dimethylaminopyridine) in sequence, stir to dissolve, and cool to -5°C in an ice bath. Add 42g of acetyl chloride into the separatory funnel, and slowly add it dropwise while stirring. Control the dropping process for 25-35min, and the temperature is lower than 10°C. After the dropwise addition, the mixture was stirred at room temperature for 2.5 h to obtain the X1 reaction solution.

[0028] Distill the reaction solution X1 under reduced pressure to control the pressure to -0.09Mpa. When the temperature rises to 51°C, pass the effluent acetyl chloride into water. When the temperature rises to 92°C, collect the effluent pyridine and recover it for use. A solid containing X1 precipitated out.

[0029] Add the obtained X1 solid into a flask containing 140 g of distilled water, stir for 40 min, and suction filter at room temperature to obtain a solid containing X1.

[0030] Add the s...

Embodiment 2

[0033] In a 500ml three-necked flask, add 240g of pyridine, 20g of guanine, and 1g of DMAP (4-dimethylaminopyridine) in sequence, stir to dissolve, and cool to -5°C in an ice bath. Add 42g of acetyl chloride into the separatory funnel, and slowly add it dropwise while stirring. Control the dropping process for 25-35min, and the temperature is lower than 10°C. After the dropwise addition, the mixture was stirred at room temperature for 2.5 h to obtain the X1 reaction solution.

[0034] Distill the reaction solution X1 under reduced pressure to control the pressure to -0.09Mpa. When the temperature rises to 51°C, pass the effluent acetyl chloride into water. When the temperature rises to 92°C, collect the effluent pyridine and recover it for use. A solid containing X1 precipitated out.

[0035] Add the obtained X1 solid into a flask containing 140 g of distilled water, stir for 40 min, and suction filter at room temperature to obtain a solid containing X1.

[0036] Add the s...

Embodiment 3

[0039] In a 500ml three-necked flask, add 240g of pyridine, 20g of guanine, and 1g of DMAP (4-dimethylaminopyridine) in sequence, stir to dissolve, and cool to -5°C in an ice bath. Add 42g of acetyl chloride into the separatory funnel, and slowly add it dropwise while stirring. Control the dropping process for 25-35min, and the temperature is lower than 10°C. After the dropwise addition, the mixture was stirred at room temperature for 2.5 h to obtain the X1 reaction solution.

[0040] Distill the reaction solution X1 under reduced pressure to control the pressure to -0.09Mpa. When the temperature rises to 51°C, pass the effluent acetyl chloride into water. When the temperature rises to 92°C, collect the effluent pyridine and recover it for use. A solid containing X1 precipitated out.

[0041] Add the obtained X1 solid into a flask containing 140 g of distilled water, stir for 40 min, and suction filter at room temperature to obtain a solid containing X1.

[0042] Add the s...

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Abstract

The invention belongs to the technical field of chemistry, and in particular, relates to a preparation method of N2,9-diacetylguanine. The method comprises the steps: A, dissolving guanine in pyridine under the condition of stirring, then adding a 4-dimethylamino pyridine DMAP catalyst into a guanine pyridine solution, cooling to -5+ / -1 DEG C, slowly dropping an acylating agent acetyl chloride, and in the dropping process, controlling the temperature to be lower than 10 DEG C; and after dropping is finished, carrying out a reaction for 2-4 h at room temperature, to obtain an X1-containing reaction liquid; B, heating the X1 reaction liquid, carrying out reduced pressure distillation to remove substances X2 and X3, and separating out an X1-containing solid; C, washing the X1-containing solid obtained in the step B with distilled water, and filtering to remove X4 and X5; and D, dissolving the X1-containing solid obtained in the step C in an acetic acid solution through stirring, and filtering to remove an undissolved substance X6, to obtain an X1-containing filtrate. The total yield of N2,9-diacetylguanine reaches 90.2%, and the purity of the product reaches 99.5%.

Description

technical field [0001] The invention belongs to the field of chemical technology, in particular to a kind of N 2 , The preparation method of 9-diacetylguanine. Background technique [0002] N 2 , 9-Diacetylguanine is an important organic and pharmaceutical synthesis intermediate, mainly used in the synthesis of antiviral drugs, such as acyclovir. Currently, industrially synthesized N 2 , 9-Diacetylguanine is mainly synthesized by using acetic anhydride as an acylating agent, guanine as a raw material, and glacial acetic acid as a solvent. This method has the advantages of low toxicity and simple operation, but the reaction needs 18 to 23 hours, the temperature requires 120° C., and the reaction conversion rate only reaches 60%. Contents of the invention [0003] For the above technical problems, the technical problem to be solved in the present invention is to provide a kind of high yield, short reaction time, low energy consumption N 2 , The preparation method of 9...

Claims

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Application Information

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IPC IPC(8): C07D473/18
CPCC07D473/18
Inventor 梁丽嫦龚美义徐珍珍陈攀崔锦栋朱文佳伍金兰李铨伍文锋朱耀框杨艳庆
Owner STAR LAKE BIOSCI CO INC ZHAOQING GUANGDONG
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