Preparation method of 2-amino-4, 6-dimethoxy pyrimidine

A technology of dimethoxypyrimidine and dimethoxypropanediamidine, which is applied in the field of preparation of 2-amino-4,6-dimethoxypyrimidine, can solve potential safety hazards, product instability when exposed to heat, and dust deterioration. Operating environment and other issues, to achieve the effect of less waste, significant social and economic benefits, and cheap raw materials

Active Publication Date: 2015-12-09
HUBEI HUIDA HIGH TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The method adopts the basic chemical raw material malononitrile as the starting raw material, adopts an improved solvent-free method in the aromatization and ring-closure step, and successfully solves the problem existing in the post-treatment process of the intermediate dimethyl cyanomalonimide The product is unstable when exposed to heat, a large amount of dust is easily generated during drying, the operating environment is deteriorated, and the safety hazards that are prone to spontaneous combustion are other key issues.

Method used

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  • Preparation method of 2-amino-4, 6-dimethoxy pyrimidine

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Embodiment 1

[0030] 1. Preparation of Dimethoxypropanediamidine (ADMP01)

[0031] In a 3000L glass-lined kettle, add metered 1800L toluene and catalyst 10kg (DMF) through the head tank, start stirring, turn on frozen brine, and cool down to below -5°C; then add the prepared malononitrile-methanol into the kettle Solution (200kg malononitrile and 300L methanol), open the dried hydrogen chloride ventilation valve, pass hydrogen chloride into the kettle, control the temperature at no more than 25°C, react for 10 hours, and take samples for central control; after the central control is qualified, put in the next step response.

[0032] 2. Preparation of 3-amino-3-methoxy-N-cyano-2-propionamidine (ADMP02)

[0033] In a 3000L glass-lined kettle, add 1000L of water, 510kg of cyanamide with a mass concentration of 30%, 1kg of disodium hydrogen phosphate and 350kg of sodium bicarbonate, cool down to -5°C, and prepare the 1,3-dimethoxy Slowly put the propylenediimine dihydrochloride solution into ...

Embodiment 2

[0040] 1. Preparation of Dimethoxypropanediamidine (ADMP01)

[0041] In a 3000L glass-lined kettle, add metered 1800L dichloroethane and catalyst 10kg (DMSO) through the head tank, start stirring, turn on frozen brine, and cool down to below -5°C; then add the prepared propanediol into the kettle Nitrile-methanol solution (200kg malononitrile and 300L methanol), open the dried hydrogen chloride ventilation valve, pass hydrogen chloride into the kettle, control the temperature at no more than 25°C, react for 15 hours, and take samples for central control; after the central control is qualified , put into the next step reaction.

[0042] 2. Preparation of 3-amino-3-methoxy-N-cyano-2-propionamidine (ADMP02)

[0043] In the 3000L glass-lined still, add 1000L water, 510kg mass concentration and be 30% cyanamide, 1kg disodium hydrogen phosphate and 350kg sodium bicarbonate, be cooled to-5 ℃, the 1,3-dimethoxy that last step is prepared Put the propylenediimine dihydrochloride solu...

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Abstract

The invention relates to the technical field of synthesis of an important midbody of medicine and chemicals, and particularly relates to a preparation method of 2-amino-4, 6-dimethoxy pyrimidine. According to the method, malononitrile is used as a basic raw material, a target object is prepared by virtue of reaction such as imidization, cyanamide substitution, aromatization cyclization and the like, particularly an aromatization cyclization optimization process is innovatively designed, so that the preparation method has characteristics of high yield, high purity and low cost. The improved process is simple in procedures, easy to industrialize, smooth to operate, less in waste gas, waste water and waste residue and environment-friendly, has remarkable social benefit and economic benefit and is suitable for industrialized production.

Description

field of invention [0001] The invention relates to the technical field of synthesis of important intermediates of medicines and pesticides, in particular to a preparation method of 2-amino-4,6-dimethoxypyrimidine. Background of the invention [0002] 2-Amino-4,6-dimethoxypyrimidine (ADMP) is one of the representatives of excellent pyrimidine compounds. It can be used as an intermediate to synthesize many kinds of pesticides. It is a super efficient sulfonylurea herbicide nicosulfuron (Nicosulfuron), Bensulfuron (Bensulfuron), Pyrazosulfuron (Pyrazosulfuron), Flazasulfuron (Flazasulfuron) and other 16 varieties of intermediates. [0003] At present about ADMP preparation method mainly contains: 1) dimethyl (ethyl) malonate and guanidine salt are raw material method (Xibei Daxue Xuebao, Ziran Kexueban, 32 (2), 145-147, 2002; Youji Huaxue, 23 (1), 106- 109,2003; JingxiYuZhuanyongHuaxuepin, 12(15),11-12,23,2006); 2) Using dimethyl (ethyl) malonate and thiourea as raw materials ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/52
CPCC07D239/52
Inventor 李永芳凌云王中奎
Owner HUBEI HUIDA HIGH TECH CO LTD
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