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A kind of synthetic method of 4,6-dimethoxy-2-((phenoxycarbonyl)amino)-pyrimidine

A technology of dimethoxypyrimidine and phenoxycarbonyl, which is applied in the field of synthesis of 4,6-dimethoxy-2-amino)-pyrimidine, can solve the problem of increasing production cost, increasing the amount of phenyl chloroformate, and three wastes Pollution increase and other problems, to achieve the effect of reducing waste water discharge, reducing production costs and improving production efficiency

Active Publication Date: 2015-09-09
INSIGHT FINECHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Yet this method can cause the content of another kind of impurity N,N-di(phenoxycarbonyl)-2-amino-4,6-dimethoxypyrimidine to increase, thereby affecting the purity of DPAP finished product; And in this method Significantly increased the amount of phenyl chloroformate, the unreacted raw material phenyl chloroformate is difficult to recover, the production cost is also increased, a large amount of phenol-containing wastewater is produced, and the corresponding three wastes pollution is increased. This route does not have practical industrial significance

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add 2-amino-4,6-dimethoxypyrimidine (500.0g / 3.23mol) to a 5000ml flask, dissolve it with 1500ml 1,4-dioxane, add N,N-dimethylaniline (640ml / 4.8mol) and DMAP (7.8g), stir and mix, slowly add phenyl chloroformate (750g / 4.80mol), control the temperature of the reaction solution not to exceed 40 ℃, stir the mixture at 35 ℃ for 7 hours, stop the reaction, the reaction mixture Slowly add 1500ml of water at 40℃ to precipitate crystals, stir for 30 minutes to make slurry, after filtration, the crude product is further purified with 50% 1,4-dioxane solution 1000ml at a temperature below 30℃, filtered and dried to obtain 834.0g of product , The content is 99.4%, and the yield is 93.8%.

[0018] The filtered mother liquor and the purified mother liquor are combined to adjust the pH to neutral, and then 600g of sodium chloride is added for salting out, and the organic layer 1,4-dioxane is separated, and the organic layer is distilled to remove water, and the water content is qualifie...

Embodiment 2

[0020] Add 2-amino-4,6-dimethoxypyrimidine (500.0g / 3.23mol) to a 5000ml flask, dissolve it with 1500ml dimethyl carbonate, and add N,N-dimethylaniline (640ml / 4.8mol) And DMAP (16.0g), stir and mix well, slowly add phenyl chloroformate (750g / 4.80mol), control the temperature of the reaction solution not to exceed 40℃, stir the mixture at 35℃ for 8h, stop the reaction, and put the reaction mixture at 40℃ Slowly add 1500ml of water to precipitate crystals, stir for 30 minutes to make a slurry. After filtration, the crude product is further purified with 1000ml of 70% dimethyl carbonate solution at a temperature below 30℃. After filtration and drying, the product 814.5g is obtained with a content of 99.3% and a yield. 91.6%.

[0021] The filtered mother liquor and the purified mother liquor are combined to adjust the pH to neutral, then 600g calcium chloride is added, the organic layer dimethyl carbonate is separated by salting out, the organic layer is distilled to remove water, and...

Embodiment 3

[0023] Add 2-amino-4,6-dimethoxypyrimidine (500.0g / 3.23mol) to a 5000ml flask, dissolve it with 2000ml methyltetrahydrofuran, add N,N-dimethylaniline (640ml / 4.8mol) and DMAP (7.8g), stir and mix, slowly add phenyl chloroformate (750g / 4.80mol), control the temperature of the reaction solution not to exceed 40℃, stir the mixture at 35℃ for 8h, stop the reaction, and put the reaction mixture at 40℃ Slowly add 1500ml of water to precipitate crystals and stir for 30 minutes to make slurry. After filtration, the crude product is further purified with 60% methyltetrahydrofuran solution 1000ml at a temperature below 30℃. After filtration and drying, 825.2g of product is obtained, with a content of 99.2% and a yield of 92.8% .

[0024] The filtered mother liquor and the purified mother liquor are combined to adjust the pH to neutral, then 500g sodium chloride is added, the organic layer methyltetrahydrofuran is separated by salting out, the organic layer is distilled to remove water, and ...

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PUM

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Abstract

The invention provides a synthesis method for 4,6-dimethoxy-2-((phenoxy carbonyl) amino)-pyrimidine. According to the method, 2-amino-4,6-dimethoxy pyrimidine and phenyl chloroformate are used as raw materials, 1,4-dioxane, dimethyl carbonate or methyl tetrahydrofuran is used as a solvent, and in the presence of N,N-dimethylaniline, 4-(N,N- dimethylamino) pyridine (DMAP) is as a catalyst. The method disclosed by the invention is mild in reaction conditions; the average purity and yield of obtained products are high; and the recovery of the solvent is simple, so that the treatment pressure of the three wastes is small, and the production cost is further reduced.

Description

Technical field [0001] The invention relates to a method for synthesizing 4,6-dimethoxy-2-((phenoxycarbonyl)amino)-pyrimidine (DPAP). DPAP is a method for preparing sulfonylurea herbicides An important intermediate of sulfuron-methyl and pyrazosulfuron-methyl. Since the purity of DPAP directly affects the purity and quality of its downstream preparation of sulfonylurea herbicides, the preparation technology of high-purity DPAP is one of the important technologies for producing qualified or high-purity sulfonylurea herbicides. Background technique [0002] The intermediate used for the herbicide preferably does not have a large amount of impurities, especially the impurities that will be carried into the final herbicide itself. Impurities in agricultural products are subject to strict regulatory inspections and are subject to strict restrictions. The advantageous method for preparing the intermediate must not only be conducive to producing high yields, but also conducive to the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D239/52
CPCC07D239/52
Inventor 凌云李永芳王中奎
Owner INSIGHT FINECHEM
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