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A kind of preparation method of 2-amino-4,6-dichloro-5-carboxamidopyrimidine

A technology of formamide and pyrimidine, which is applied in the field of compound preparation, can solve the problems of difficult removal of phosphorus-containing wastewater, difficulty in large-scale production operations, and difficulty in qualified discharge, and achieves the effects of being beneficial to industrialized production, improving safety, and improving efficiency.

Active Publication Date: 2021-02-09
SUZHOU KAIYUAN MINSHENG SCI & TECH CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Such as CN201610555849.4, however, this method causes too many by-products during hydrolysis, and the phosphorus-containing wastewater produced is difficult to remove, and it is difficult to discharge qualifiedly in production
Chlorination and hydrolysis conditions are not described in detail in CN103936681, it is difficult to master it, and it is even more difficult to carry out large-scale production operations

Method used

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  • A kind of preparation method of 2-amino-4,6-dichloro-5-carboxamidopyrimidine
  • A kind of preparation method of 2-amino-4,6-dichloro-5-carboxamidopyrimidine
  • A kind of preparation method of 2-amino-4,6-dichloro-5-carboxamidopyrimidine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0075] Synthesis of Nitrosomalononitrile (I), Nitrosoformamidine (III)

[0076] Add 165.0g (2.5mol) of malononitrile and 825g of 25% hydrochloric acid into a 2000mL four-necked reaction flask, start stirring, cool down to 0°C, add 593g of 35% sodium nitrite solution dropwise, and react at room temperature for 2 hours (detection The raw material was HPLC<0.3%), cooled to 5°C, filtered and dried by suction to obtain 235.1 g of a solid, the purity of which was measured by HPLC was 99.5%, and the yield was 99.0% (calculated as malononitrile).

[0077] Add 201.3g (2.5mol) of formamidine hydrochloride and 1005g of 25% hydrochloric acid into a 2000mL four-necked reaction flask, start stirring, cool down to 0°C, add 593g of 35% sodium nitrite solution dropwise, and react at room temperature for 2 hours (detection Raw material HPLC<0.3%), cooled to 5°C, suction filtered and dried to obtain 181.0 g of solid, the purity measured by HPLC was 99.5%, and the yield was 99.2% (calculated as f...

Embodiment 2

[0079] Synthesis of formamidomalononitrile (II)

[0080] Add 230g (2.42mol) of nitrosomalononitrile, 690.0g formic acid, and 95.0g iron powder into a 1000mL four-necked reaction flask, stir, heat up to 100°C and reflux for 4 hours (HPLC for detection of raw materials<0.5%), cool down to Filtrate at 50°C, apply the filter cake (KF detection is below 0.5%), distill formic acid from the filtrate under reduced pressure until the solid precipitates, then slowly cool down to 0°C, filter and dry to obtain 251.0 g of solid, the purity of which is 99.0% by HPLC. The yield was 95.2%.

Embodiment 3

[0082] Synthesis of formamidomalononitrile (II)

[0083] Add 230g (2.42mol) of nitrosomalononitrile, 690.0g formic acid, and 110.0g zinc powder into a 1000mL four-necked reaction flask, stir, heat up to 100°C and reflux for 4 hours (HPLC for detection of raw materials<0.5%), cool down to Filtrate at 50°C, apply the filter cake (KF detection is less than 0.5%), distill formic acid from the filtrate under reduced pressure until the solid precipitates, then slowly cool down to 0°C, filter and dry to obtain 252.0g of solid, the purity of which is 99.1% by HPLC. The yield was 95.5%.

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Abstract

The invention provides a preparation method of 2-amino-4,6-dichloro-5-carboxamidopyrimidine. The preparation method comprises using malononitrile, formamidine or its hydrochloride as starting materials, and preparing 2-amino-4 through nitrosation, formylation, cyclization, diazotization, Sandmeyer and reduction reactions. ,6-Dichloro-5-carboxamidopyrimidine. The production rate of the preparation method of the invention is high while the product purity is high.

Description

technical field [0001] The invention relates to a preparation method of 2-amino-4,6-dichloro-5-carboxamidopyrimidine, which belongs to the technical field of compound preparation. Background technique [0002] According to the report of the World Health Organization, since the discovery and reporting of AIDS in 1981, there have been a total of 69 million infected people worldwide, of which 40% have died. Now there are more than 5 million new HIV infection cases every year. At present, the total number of HIV / AIDS patients has reached There are more than 42 million people. If effective prevention and control are not implemented, it is estimated that the number of HIV-infected people will reach 200 million in 20 years. [0003] Abacavir is a new anti-AIDS drug. It is a new carbocyclic 2'-deoxyguanosine nucleoside drug. It has high oral bioavailability and is easy to penetrate into the central nervous system. The drug is a nucleoside reverse transcriptase preparation approved ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D239/48
CPCC07D239/48
Inventor 高鹏黄忠林孙思徐剑锋曾淼
Owner SUZHOU KAIYUAN MINSHENG SCI & TECH CORP