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Synthesis 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 high operating cost, low cost, poor quality of anhydrous hydrogen chloride, etc., and achieve The effect of high yield, low moisture control and stable product quality

Active Publication Date: 2018-03-06
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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  • Synthesis method of 2-chloro-4,6-dimethoxypyrimidine
  • Synthesis method of 2-chloro-4,6-dimethoxypyrimidine
  • Synthesis method of 2-chloro-4,6-dimethoxypyrimidine

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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 drip 235.5g of acetyl chloride into the kettle, control the reaction temperature at 0-5°C, and the dripping time for 5 hours. After the dripping is completed, continue the insulation reaction 1 After hours, it is filtered under nitrogen protection to obtain 1,3-dimethylmalonamide dihydrochloride wet product.

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

[0024] Add 1,3-dimethylmalonamide dihydrochloride and lye (sodium bicarbonate 20g, sodium hydroxide 30g, water 500g) to the reaction kettle, control the reaction temperature at -5-0℃, and slowly add to the solution 110g 50% cyanamide solution, pH value of the reaction is 5-7, the molar ratio of the feed is that after the feed is completed, the temperature in the kettle is slowly raised to 18℃, kept for 10 hours, filtered, washed, and dried to obtain...

Embodiment 2

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

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

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

[0032] Add 1,3-dimethylmalonamide dihydrochloride and lye (20g sodium bicarbonate, 30g sodium hydroxide, 500g water) to the reaction kettle, control the reaction temperature at 0-3℃, and slowly add 50 to the solution % Cyanamide solution 101g, the reaction pH value is 7.5-8, the molar ratio of the feed is that after the feed is completed, the temperature in the kettle is slowly raised to 27°C, kept for 10 hours, filtered, washed, and dried to obtain 3-...

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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 method for synthesizing 2-chloro-4,6-dimethoxypyrimidine and belongs to the technical field of organic synthesis. Background technique [0002] In the development of pesticides, heterocyclic compounds have become the mainstream of new pesticide research and development. Pyrimidine compounds are an important class of biologically active substances, which are widely used in pesticides, 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, the synthetic method of 2-chloro-4,6-dimethoxypyrimidine uses malononitrile as a raw material to have a lower cost. Currently, malononitrile, methanol, anhydrous hydrogen chloride, toluene, cyanamide, and carbonic acid are used. The syntheti...

Claims

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Application Information

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Patent Type & Authority Applications(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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