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The synthetic method of 2-chloro-4,6-dimethoxypyrimidine

A dimethoxypyrimidine and synthesis method technology, applied in the field of synthesis of 2-chloro-4,6-dimethoxypyrimidine, can solve the problems of low cost, high operating cost, and poor quality of anhydrous hydrogen chloride, and achieve The effect of low moisture control, high yield and stable product quality

Active Publication Date: 2020-05-19
YINGKOU YINGXIN CHEM TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, in the synthetic method of 2-chloro-4,6-dimethoxypyrimidine, the cost of the synthetic route using malononitrile as raw material is relatively low. At present, malononitrile, methanol, anhydrous hydrogen chloride, toluene, cyanamide, carbonic acid The synthesis route of sodium hydrogen raw material, the intermediate 1,3-dimethylmalonimidine dihydrochloride is absolutely anhydrous during the synthesis process, wherein anhydrous hydrogen chloride gas is one of the necessary raw materials, but there are preparations of anhydrous hydrogen chloride, The drying equipment is complicated, the operating cost is high, and the quality of anhydrous hydrogen chloride directly affects the product yield and other issues

Method used

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  • The synthetic method of 2-chloro-4,6-dimethoxypyrimidine
  • The synthetic method of 2-chloro-4,6-dimethoxypyrimidine
  • The synthetic method of 2-chloro-4,6-dimethoxypyrimidine

Examples

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Embodiment 1

[0021] (1) Synthesis of 1,3-dimethylmalonamide dihydrochloride

[0022] Put 66g of malononitrile and 176g of anhydrous methanol into the reaction kettle, slowly drop 235.5g of acetyl chloride into the kettle, control the reaction temperature at 0-5°C, and add the time for 5 hours. After the addition, continue the insulation reaction for 1 Hour, nitrogen protection filtration, obtains 1,3-dimethylmalonamidine dihydrochloride wet product.

[0023] (2) Synthesis of 3-amino-3-methoxy-N-cyano-2-propionamidine

[0024] Add 1,3‐dimethylmalonimidine dihydrochloride and lye (sodium bicarbonate 20g, sodium hydroxide 30g, water 500g) into the reaction kettle, control the reaction temperature -5-0°C, and slowly add 110g of 50% cyanamide solution, the reaction pH value is 5-7, and the molar ratio of feeding is such that the temperature in the kettle slowly rises to 18°C ​​after the feeding is completed, and the temperature is kept at 10 hours, filtered, washed, and dried to obtain 3-amino...

Embodiment 2

[0029] (1) Synthesis of 1,3-dimethylmalonimidine dihydrochloride

[0030] Put 66g of malononitrile and 204.8g of anhydrous methanol into the reaction kettle, slowly drop 353.25g of acetyl chloride into the kettle, control the reaction temperature at 10-15°C, and add the time for 8 hours. After the addition, continue the insulation reaction After 2 hours, filter under nitrogen protection to obtain the wet product of 1,3-dimethylmalonamidine dihydrochloride.

[0031] (2) Synthesis of 3-amino-3-methoxy-N-cyano-2-propionamidine

[0032] Add 1,3‐dimethylmalonimidine dihydrochloride and lye (sodium bicarbonate 20g, sodium hydroxide 30g, water 500g) into the reaction kettle, control the reaction temperature at 0-3°C, and slowly add 50 % cyanamide solution 101g, the reaction pH value is 7.5-8, and the molar ratio of feeding is such that the temperature in the kettle slowly rises to 27°C after the feeding is finished, and it is kept for 10 hours, filtered, washed, and dried to obtain ...

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Abstract

The invention provides a synthesis method of 2-chloro-4,6-dimethoxypyrimidine and belongs to the technical field of organic synthesis. A synthesis route that malononitrile, methanol, acetyl chloride,hydrogen cyanamide and alkali liquor are taken as raw materials is adopted, malononitrile is dropwise added into a system of malononitrile and methanol, 1,3-dimethamidine dihydrochloride is directly obtained, then reaction is carried out with sodium bicarbonate and hydrogen cyanamide to obtain 3-amino-3-methoxy-N-nitrile-2-propyl amidine, and further reaction is carried out with hydrogen chloride,so that 2-chloro-4,6-dimethoxypyrimidine is obtained. The synthesis method provided by the invention has the advantages that tedious synthesis process and equipment of 1,3-dimethamidine dihydrochloride are eliminated, acetyl chloride is added into the malononitrile and methanol, and 1,3-dimethamidine dihydrochloride is directly obtained by virtue of a one-step method. The synthesis route of 1,3-dimethamidine dihydrochloride has the advantages that moisture is controlled to be extremely low, product quality is stable and yield is high.

Description

technical field [0001] The invention relates to a synthesis method of 2-chloro-4,6-dimethoxypyrimidine, which belongs to the technical field of organic synthesis. Background technique [0002] In the development of pesticides, heterocyclic compounds have become the mainstream of research and development of new pesticides. Pyrimidine compounds are an important class of biologically active substances, which are widely used in insecticides, herbicides, fungicides and pharmaceutical intermediates and have attracted people's attention. In the production of sulfonylurea herbicides, 2-chloro-4,6-dimethoxypyrimidine is an important intermediate in its synthesis, and there are many varieties of sulfonylurea herbicides prepared from it. [0003] At present, in the synthetic method of 2-chloro-4,6-dimethoxypyrimidine, the cost of the synthetic route using malononitrile as raw material is relatively low. At present, malononitrile, methanol, anhydrous hydrogen chloride, toluene, cyanami...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D239/52
CPCC07D239/52
Inventor 刘至寻梁海张佳兴陈光强宋颖尹诗李志国丁一
Owner YINGKOU YINGXIN CHEM TECH CO LTD
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