Preparation method of 2-amino-4, 6-dichloro-5-formamidopyrimidine

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, difficult large-scale production operation, and difficult discharge of qualified standards, and achieves the effects of industrial production, improved safety, and improved efficiency

Active Publication Date: 2020-12-11
SUZHOU KAIYUAN MINSHENG SCI & TECH CORP
View PDF8 Cites 2 Cited by
  • 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 qualif

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of 2-amino-4, 6-dichloro-5-formamidopyrimidine
  • Preparation method of 2-amino-4, 6-dichloro-5-formamidopyrimidine
  • Preparation method of 2-amino-4, 6-dichloro-5-formamidopyrimidine

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%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention provides a preparation method of 2-amino-4, 6-dichloro5formyl pyrimidine. The preparation method comprises the following steps: by taking malononitrile, formamidine or hydrochloride thereof as initial raw materials, carrying out nitrosation, formylation, cyclization, diazotization, Sandmeyer and reduction reaction to prepare the 2-amino-4, 6-dichloro-5-formamidopyrimidine. The preparation method disclosed by the invention is high in yield and high in product purity.

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
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
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap