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Method for effectively reducing nickel remaining in 2,4,5-triamino-6-hydroxypyrimidinesulfate

A technology of hydroxypyrimidine and triamino, which is applied in the field of preparation of anti-herpes drugs, can solve problems affecting product yield and product loss, and achieve good temperature stability, reduced hazards, good storage stability and operational safety.

Inactive Publication Date: 2016-12-07
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

[0013] Because this kind of method is beating or flushing after the final product is formed, it will cause a large amount of waste water, and the waste water will contain a large amount of nickel, which will also cause product loss, affect the product yield, and bring great environmental protection and economy. stress and burden

Method used

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  • Method for effectively reducing nickel remaining in 2,4,5-triamino-6-hydroxypyrimidinesulfate
  • Method for effectively reducing nickel remaining in 2,4,5-triamino-6-hydroxypyrimidinesulfate

Examples

Experimental program
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Effect test

Embodiment ( 1

[0028] Add 56.3g of 2,4-diamino-5-nitroso-6-hydroxypyrimidine into the hydrogenation kettle, then add 800-1000g of water, start stirring, add 12-14g of sodium hydroxide, adjust ph=12-13 , then add 0.51g of active nickel, start stirring, replace the vacuum with nitrogen for 3 times, then replace the vacuum with hydrogen for 3 times, fill in hydrogen to make the pressure rise to 0.2-0.24Mpa, raise the temperature to 68 degrees, when the pressure rises to 0.4- Turn off the hydrogen at 0.42Mpa, stir for 1-2min, the pressure does not drop significantly, the temperature in the reactor is 85-90 degrees, filter and separate, add 0.31g organic sulfur polymer heavy metal scavenger TMT10 to the filtrate, heat to 70-80 degree, stirred for 65min, hot filtered, added dropwise 70-80g of 50% sulfuric acid to the green leaves for acidification, adjusted the pH to between 1-2, continued to stir for 20min, filtered, and dried to obtain light yellow 2,4,5- Triammonium 6-hydroxypyrimidine sulfate ...

Embodiment ( 2

[0030] Add 56.5g of 2,4-diamino-5-nitroso-6-hydroxypyrimidine into the hydrogenation kettle, then add 800-1000g of water, start stirring, add 12-14g of sodium hydroxide, adjust ph=12-13 , then add 0.5g of active nickel, start stirring, replace the vacuum with nitrogen for 3 times, then replace the vacuum with hydrogen for 3 times, fill in hydrogen to make the pressure rise to 0.2-0.24Mpa, raise the temperature to 68 degrees, when the pressure rises to 0.4- Turn off the hydrogen at 0.42Mpa, stir for 1-2min, the pressure does not drop significantly, the temperature in the reactor is 85-90 degrees, filter and separate, add 0.26g organic sulfur polymer heavy metal scavenger TMT18 to the filtrate, heat to 70-80 degree, stirred for 90min, hot filtered, added dropwise 70-80g of 50% sulfuric acid to the green leaves for acidification, adjusted the pH to between 1-2, continued to stir for 20min, filtered, and dried to obtain light yellow 2,4,5- 72.9 g of triamino-6-hydroxypyrimidine su...

Embodiment ( 3

[0032] Add 56.3g of 2,4-diamino-5-nitroso-6-hydroxypyrimidine into the hydrogenation kettle, then add 800-1000g of water, start stirring, add 12-14g of sodium hydroxide, adjust ph=12-13 , then add 0.52g of active nickel, start stirring, replace the vacuum with nitrogen for 3 times, then replace the vacuum with hydrogen for 3 times, fill in hydrogen to make the pressure rise to 0.2-0.24Mpa, raise the temperature to 68 degrees, when the pressure rises to 0.4- Turn off the hydrogen at 0.42Mpa, stir for 1-2min, the pressure does not drop significantly, the temperature in the reactor is 85-90 degrees, filter and separate, add 0.29g organic sulfur polymer heavy metal scavenger EDTC to the filtrate, heat to 70-80 degree, stirred for 85min, filtered hot, added dropwise 70-80950% sulfuric acid to the green leaves for acidification, adjusted the pH to between 1-2, continued to stir for 20min, filtered, and dried to obtain light yellow 2,4,5- 71.8g of triamino-6-hydroxypyrimidine sulfate...

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Abstract

The invention relates to a method for effectively reducing nickel remaining in 2,4,5-triamino-6-hydroxypyrimidinesulfate. The method is characterized in that the 2,4-diamino-5-nitroso-6-hydroxypyrimidine is used as a raw material, under the alkaline condition, hydrogen is led, and nickel is used as a catalyst, so that catalytic hydrogenation reduction is performed; after the reaction is completed, a hydrogenation mother solution is transferred, nitrogen is used for protection, a spin trapping agent of heavy metal nickel is added, and a complexing reaction is performed, so that an insoluble remainder precipitation which is non-toxic, harmless, stable, and environmental-friendly is generated; and filtration is performed, and acidification is performed, so that the 2,4,5-triamino-6-hydroxypyrimidinesulfate is prepared. The method disclosed by the invention has a main progress that the nickel residue in the 2,4,5-triamino-6-hydroxypyrimidinesulfate is effectively reduced, and the method is an economic and environmental-friendly cleaning technology.

Description

technical field [0001] The invention relates to a preparation method of an anti-herpes drug with high efficiency and low toxicity, in particular to a preparation method of 6-hydroxy-2,4,5-triaminopyrimidine sulfate, acyclovir, famciclovir and other drugs, belonging to medicine and chemical industry technology field. Background technique [0002] Chemical name: 6-hydroxyl-2,4,5-triaminopyrimidine sulfate, structural formula (I) is as follows: [0003] [0004] It is an important intermediate of a series of high-efficiency and low-toxic anti-herpes drugs such as acyclovir and famciclovir. Because acyclovir is an anti-herpes drug with high efficiency and low toxicity, it has a broad market prospect, and has attracted extensive attention from various medical circles. Reports on salt preparation methods. [0005] Its preparation process is roughly divided into the following steps: [0006] (1) ring closure. Methyl cyanoacetate and guanidine nitrate are cyclized to generat...

Claims

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Application Information

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IPC IPC(8): C07D239/50
CPCC07D239/50
Inventor 孔立楚玮明程焕达徐汉青刘勇军朱钦朋
Owner 江苏八巨药业有限公司
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