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Preparation method of 6-hydroxy-2, 4, 5-triaminopyrimidine sulfate

A technology of triaminopyrimidine and sulfate, applied in the fields of medicine and chemical industry, can solve the problems of easily causing product quality risks, poor stability of guanidine hydrochloride, and increasing production costs, and achieves the effect of avoiding reaction safety risks and being beneficial to sustainable development.

Pending Publication Date: 2022-05-24
江苏八巨药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Historically, the research on the cyclization was mainly carried out through guanidine nitrate or guanidine hydrochloride. Since guanidine nitrate contains nitrate and guanidine hydrochloride contains halogen salts, a large amount of sodium nitrate or sodium chloride will be produced during the cyclization reaction. , and brought into the nitrosation reaction, a large amount of high-nitrogen or high-chlorine wastewater will be produced, which will bring great pressure to environmental protection treatment. At the same time, because guanidine nitrate contains nitro, it is an explosive and has a high safety risk. Guanidine hydrochloride Poor stability, easy to absorb moisture, easy to cause product quality risks, reduce product yield, and increase production costs

Method used

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  • Preparation method of 6-hydroxy-2, 4, 5-triaminopyrimidine sulfate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] (1) 40 g of guanidine sulfate was added to 100 g of methanol, then 41 g of solid sodium methoxide was added, the temperature was raised to 60° C. with stirring, and the mixture was freed for 1 hour. Then, 37 g of methyl cyanoacetate was slowly added dropwise to the reaction solution, and the cyclization reaction was completed by refluxing for 3 hours to obtain a cyclization reaction solution.

[0038] (2) after the step (1) cyclization reaction solution is distilled to recover the solvent methanol, add 150 g of water and stir, be warming up to 80 ° C after dissolving, then be cooled to 20 ° C, dropwise the mass percentage concentration of 50% sulfuric acid 90g acidification , adjust pH to 1, set aside.

[0039] (3) 27g sodium nitrite is dissolved in the water of 40.5g, is mixed with the sodium nitrite solution that mass percent concentration is 40%, is slowly added dropwise in step (2) and reacts, the reaction temperature is 20 ℃, and the reaction end point is The nitr...

Embodiment 2

[0043] (1) 40 g of guanidine sulfate was added to 100 g of methanol, then 51.5 g of solid sodium ethoxide was added, the temperature was raised to 60° C. with stirring, and freed for 1 hour. Then, 36 g of methyl cyanoacetate was slowly added dropwise to the reaction solution, and the reflux reaction was completed for 3 hours to obtain a cyclization reaction solution.

[0044] (2) after the step (1) cyclization reaction solution is distilled to recover the solvent methanol, add 150 g of water and stir, be warming up to 80 ° C and dissolve the clear, then be cooled to 20 ° C, drop the mass percentage concentration of 90 g of sulfuric acid that is 50% Acidify, adjust pH to 1, and set aside.

[0045] (3) 27g sodium nitrite is dissolved in the water of 40.5g, is mixed with the sodium nitrite solution that the mass percent concentration is 40%, is slowly added dropwise in step (2) and reacts, the reaction temperature is 10 ℃, and the reaction end point is The nitrous solution turns...

Embodiment 3

[0049] (1) 40 g of guanidine sulfate was added to 100 g of methanol, then 73 g of solid sodium tert-butoxide was added, the temperature was raised to 60° C. with stirring, and freed for 1 hour. Then, 36 g of methyl cyanoacetate was slowly added dropwise to the reaction solution, and the reflux reaction was completed for 3 hours to obtain a cyclization reaction solution.

[0050] (2) after the step (1) cyclization reaction solution is distilled to recover the solvent methanol, add 150 g of water and stir, be warming up to 80 ° C after dissolving clear, then be cooled to 10 ° C, dropwise the mass percentage concentration of 50% sulfuric acid 90g acidification , adjust pH to 2, set aside.

[0051] (3) 27g sodium nitrite is dissolved in the water of 40.5g, is mixed with the sodium nitrite solution that mass percent concentration is 40%, is slowly added dropwise in step (2) and reacts, the reaction temperature is 20 ℃, and the reaction end point is The nitrous solution turns the s...

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Abstract

In order to solve the technical problem that in a traditional preparation method of 6-hydroxy-2, 4, 5-triaminopyrimidine sulfate, a process for cyclization by guanidine nitrate or guanidine hydrochloride is not beneficial to safety, environmental protection and product quality, the invention provides a novel method for preparing 6-hydroxy-2, 4, 5-triaminopyrimidine sulfate, guanidine sulfate is adopted to replace the traditional guanidine nitrate or guanidine hydrochloride, and the yield of 6-hydroxy-2, 4, 5-triaminopyrimidine sulfate is increased. The 6-hydroxy-2, 4, 5-triaminopyrimidine sulfate is prepared by cyclization with methyl cyanoacetate, nitrosation, catalytic hydrogenation and sulfuric acid acidification salification, so that sodium nitrate or sodium chloride is avoided, total nitrogen or total chlorine in subsequent wastewater is reduced, and environmental protection is facilitated. Meanwhile, the reaction safety risk caused by guanidine nitrate or the product quality risk caused by guanidine hydrochloride can be avoided, and sustainable development is facilitated.

Description

technical field [0001] The invention belongs to the technical field of medicine and chemical industry, and particularly relates to a preparation method of 6-hydroxy-2,4,5-triaminopyrimidine sulfate. Background technique [0002] Chemical name: 6-hydroxy-2,4,5-triaminopyrimidine sulfate, English name 6-Hydroxy-2,4,5-triaminopyrimidine sulfatehydrate, structural formula (Ⅰ) is shown below. [0003] [0004] It is an important intermediate of a series of high-efficiency and low-toxic anti-herpes drugs such as acyclovir and famciclovir. [0005] As acyclovir is a kind of high-efficiency and low-toxicity anti-herpes drug, it has broad market prospects and has attracted extensive attention from various medical circles. A report on the method of salt preparation. [0006] The preparation process of 6-hydroxy-2,4,5-triaminopyrimidine sulfate is roughly divided into the following steps: [0007] (1) Ring closure [0008] Methyl cyanoacetate and guanidine nitrate or guanidine h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/50
CPCC07D239/50Y02P20/584
Inventor 程焕达张进福申小科王小明周子敬
Owner 江苏八巨药业有限公司
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