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One-step synthesis method of guanine

A synthesis method and guanine technology, applied in the field of medicine, can solve the problems of difficult by-product treatment and high environmental protection treatment cost, and achieve the effects of reducing environmental protection treatment costs and eliminating potential safety hazards.

Active Publication Date: 2022-04-22
湖北李泽园医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, due to the use of liquid caustic soda, sulfuric acid and formic acid, it is difficult to treat by-products, and the cost of environmental protection treatment is high.

Method used

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  • One-step synthesis method of guanine
  • One-step synthesis method of guanine
  • One-step synthesis method of guanine

Examples

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Effect test

preparation example Construction

[0034] A kind of one-step synthetic method of guanine, it comprises:

[0035] Mix 2,4-diamino-5-nitroso-6-hydroxypyrimidine with formamide solution, raise the temperature to 80-160°C under the catalyst for formylation reaction, and then raise the temperature to 160-180°C to keep the temperature dehydration reaction.

[0036] The reaction process of this synthetic method is as follows:

[0037]

[0038] Using this process, in the synthesis process, 2,4-diamino-5-nitroso-6-hydroxypyrimidine is added to the aqueous formamide solution, and under the catalyst condition, the temperature is slowly raised, and the excess water in the formamide solution Evaporate gradually (because the boiling point of formamide is 210°C, formamide will not evaporate with water), and at the same time, initiate a formylation reaction to obtain a formamidopyrimidine transition intermediate. The transition intermediate can exist stably, and the pure intermediate monomer can be obtained by means of se...

Embodiment 1

[0050] The present embodiment provides a kind of one-step synthesis method of guanine, which comprises:

[0051]Take 31g (0.2mol) of 2,4-diamino-5-nitroso-6-hydroxypyrimidine, add it to 120ml 75% formamide, start stirring, slowly raise the temperature to 80°C, add 2.5g (about 8% ) Sodium dithionite, continue to heat up to trigger the formylation reaction, and at the same time, a large amount of ammonia and carbon dioxide gas overflow, which are absorbed by deionized water circulation. Collect the water continuously evaporated during the heating process, and raise the temperature to 160°C within 7 hours to complete the formylation reaction. Continue to heat up, when the temperature rises to 170°C, stop the water outlet, reflux and keep warm for 2 hours, cool down after the material turns yellow, and filter to obtain crude guanine with a yield of about 99%.

[0052] The crude product was added into 10 times 15% dilute hydrochloric acid to reflux for decolorization and refinemen...

Embodiment 2

[0055] The present embodiment provides a kind of one-step synthesis method of guanine, which comprises:

[0056] Take 60g of 2,4-diamino-5-nitroso-6-hydroxypyrimidine wet product, convert it to 31g (0.2mol), add it to 120ml of 80% formamide, start stirring, slowly heat up to 80°C, add 2.0 g (about 6.5%) sodium dithionite, continue to heat up to trigger the formylation reaction, and a large amount of ammonia and carbon dioxide gas overflow at the same time, and are absorbed by deionized water circulation. Collect the water continuously evaporated during the heating process, and raise the temperature to 160°C within 6 hours to complete the formylation reaction. When the temperature rises to 160° C., stop the water outlet, reflux and keep warm for 3 hours, cool down after the material turns yellow, and filter to obtain crude guanine with a yield of about 98.6%.

[0057] The crude product was added into 10 times 15% dilute hydrochloric acid to reflux for decolorization and refine...

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Abstract

The invention discloses a one-step synthesis method of guanine, and belongs to the field of biology. The synthesis method comprises the following steps: mixing 2, 4-diamino-5-nitroso-6-hydroxypyrimidine with a formamide solution, heating to 80-160 DEG C in the presence of a catalyst, carrying out formylation reaction, then heating to 160-180 DEG C, and carrying out heat preservation for dehydration reaction. The method is simple in process, hydrogenation reduction is not needed, and potential safety hazards are eliminated; and meanwhile, the use of reagents such as rare metal catalysts, alkali and formic acid is also omitted, so that the method is more environment-friendly. Meanwhile, the yield of a guanine crude product obtained through a one-step reaction in the reaction is 97% or above, a pure guanine finished product is obtained after refining, the yield can reach 90%, and the purity is larger than or equal to 99.5%.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a one-step synthesis method of guanine. Background technique [0002] Guanine is the main base component of nucleic acid and has important physiological functions. At the same time, guanine also has a lot of medicinal value. It is a pharmaceutical intermediate of traditional Chinese medicine, such as the synthetic antiviral drugs Acyclovir, Ganciclovir and other Clovir series drugs, which have great industrial production value. [0003] The traditional production process of guanine is to take methyl cyanoacetate as starting raw material, and carry out the reaction of following steps successively: [0004] (1) Condensation reaction: methyl cyanoacetate is cyclized with guanidine nitrate (or guanidine hydrochloride) to obtain 2,4-diamino-6-hydroxypyrimidine. [0005] [0006] (2) Nitrosation reaction: Nitrosation reaction with sodium nitrite to obtain 2,4-diamino-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D473/18
CPCC07D473/18Y02P20/584
Inventor 谢文建
Owner 湖北李泽园医药科技有限公司
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