Unlock instant, AI-driven research and patent intelligence for your innovation.

A kind of method for preparing 2-amino-4,6-dimethoxypyrimidine

A technology of dimethoxypyrimidine and dimethoxypropanediimine dihydrochloride, which is applied in the chemical industry and can solve the problems of unavailable raw materials of monosodium cyanamide and disodium cyanamide, human and environmental hazards, chlorobenzene Toxicity and other problems, to achieve the effect of low price, low production cost, and reduce side effects

Active Publication Date: 2018-05-11
HUBEI RUISI TECH
View PDF4 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0017] U.S. Patent No. 5,070,201 discloses that 2-amino-4,6-dimethoxypyrimidine is prepared by reacting propanediimine dihydrochloride, monosodium cyanamide, and disodium cyanamide as raw materials in solvent chlorobenzene. Although the operation is simple and the yield is high, the raw materials of monosodium cyanamide and disodium cyanamide are not easy to obtain, the price is expensive, and the toxicity of chlorobenzene is relatively high, which is seriously harmful to people and the environment.

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
  • A kind of method for preparing 2-amino-4,6-dimethoxypyrimidine
  • A kind of method for preparing 2-amino-4,6-dimethoxypyrimidine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039]Mix 406g of 1,3-dimethoxypropanediimine dihydrochloride with 1500g of toluene, add 260g of triethylamine, and add 136.5g of xanthamide to the reaction bottle under stirring, and heat it at 20~25℃ After 3 hours of reaction, the reaction is completed, and the temperature is raised to perform the ring-closing reaction. At the same time, the reaction bottle is degassed with a vacuum microstrip negative pressure (-0.03MPa). Reaction, lower the temperature to 80°C, add 700g of water to the reaction flask, stir and wash, separate the liquids, and after the organic phase is subjected to precipitation treatment, high vacuum rectification (vacuum degree at 1mmHg) is carried out to obtain white 2-amino- 4,6-dimethoxypyrimidine solid weighs 280.0 g, yield 90.32%, purity: 99.85% (HPLC analysis).

Embodiment 2

[0041] Mix 406g of 1,3-dimethoxypropanediimine dihydrochloride with 2000g of xylene, add 326g of N,N-dimethylaniline, and add 147.0g of xanthamide to the reaction bottle under stirring , after reacting at 20-25°C for 3 hours, the reaction is complete, and the temperature is raised for ring-closing reaction. After being incubated for 30 minutes, stop the reaction, cool down to 80°C, add 800g of water to the reaction flask, stir and wash, separate the liquids, and after the organic phase is subjected to precipitating treatment, carry out high vacuum rectification (vacuum degree at 1mmHg) to obtain The white solid of 2-amino-4,6-dimethoxypyrimidine weighs 285.0 g, the yield is 91.9%, and the purity is 99.80% (HPLC analysis).

Embodiment 3

[0043] Mix 406g of 1,3-dimethoxypropanediimine dihydrochloride with 1800g of xylene, add 250g of trimethylamine, and add 140.0g of xanthamide to the reaction bottle under stirring, at 20~25℃ After 3 hours of reaction, the reaction is completed, and the temperature is raised to perform the ring-closing reaction. At the same time, the reaction bottle is degassed (-0.03MPa) with a vacuum micro-band negative pressure. Reaction, the temperature was lowered to 80°C, 750g of water was added to the reaction flask, stirred and washed, separated, the organic phase was subjected to precipitation treatment, and then high-vacuum rectification (vacuum degree at 1mmHg) was carried out to obtain white 2-amino- 4,6-dimethoxypyrimidine solid weighs 283.0 g, yield 91.3%, purity: 99.88% (HPLC analysis).

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 relates to the field of chemical industry, particularly a method for preparing 2-amino-4,6-dimethoxy pyrimidine. The method comprises the following steps: by using 1,3-dimethoxypropyldiimine dihydrochloride as a raw material, adding an alkali and xanthogenamide into a reaction solvent to react, thereby obtaining a material 1; and heating the material 1 to perform cyclization and degassing, thereby obtaining the synthetic target product 2-amino-4,6-dimethoxy pyrimidine.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a method for preparing 2-amino-4,6-dimethoxypyrimidine. Background technique [0002] Urea herbicides are broad-spectrum and high-efficiency herbicides for rice, corn, and soybean fields. They have high activity and a wide herbicidal spectrum. They have good stem and leaf treatment activity and certain soil sealing effect. Low residue and friendly to the environment. [0003] In the production of sulfonylurea herbicides, 2-amino-4,6-dimethoxypyrimidine is an important intermediate in its synthesis, and there are many varieties of sulfonylurea herbicides prepared by it, such as benzsulfone Nicosulfuron, Nicosulfuron, Cyprosulfuron, Ethoxysulfuron, Erimsulfuron-methyl, Acylsulfuron-methyl, Flumesulfuron-methyl, Clopyrimsulfuron-methyl, Tetrazosulfuron-methyl, Pyrazosulfuron-methyl Benzyl, sulfasulfuron-methyl, sulfasulfuron-methyl, etc. For this reason, the preparation method of...

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
Patent Type & Authority Patents(China)
IPC IPC(8): C07D239/52
CPCC07D239/52
Inventor 陈文王科肖福贵李敬冬
Owner HUBEI RUISI TECH