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Method for preparing high purity 4,6-dimethoxy-2-((phenoxy carbonyl)amido)-pyrimidine

A technology of dimethoxypyrimidine and phenoxycarbonyl, applied in the field of preparation of high-purity 4,6-dimethoxy-2-((phenoxycarbonyl)amino)-pyrimidine, which can solve the problem of increasing waste water discharge, Increase costs, affect product quality and other issues

Inactive Publication Date: 2010-12-29
JIANGSU POLYTECHNIC UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After the reaction of this method is completed, the post-treatment method of directly adding water to the reaction system to separate out the product is adopted. The solvent cannot be recovered, which not only increases the cost but also increases the discharge of waste water. The problem seriously affects the quality of the product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0004] Example 1 Put 5g (0.032mol) 2-amino-4,6-dimethoxypyrimidine on a 100ml flask, dissolve it in 10ml tetrahydrofuran, add 6.4ml (0.048mol) N, N-dimethylaniline, slowly add 6.4 ml (0.048mol) phenyl chloroformate, control the temperature of the reaction solution not to exceed 40°C, stir the mixture at 30°C for 18 hours, evaporate the solvent from the reaction mixture at 40°C under reduced pressure, add 20ml of methanol to dissolve the solid, wait until When there is no bulk solid, slowly add 30ml of water to precipitate crystals, stir for 30 minutes, and filter. 7.6g, yield 87.8%, content 98.6%.

example 2

[0005] Example 2 Put 5g (0.032mol) 2-amino-4,6-dimethoxypyrimidine on a 100ml flask, dissolve it with 10ml tetrahydrofuran, add 6.4ml (0.048mol) N, N-dimethylaniline, slowly add 6.4 ml (0.048mol) of phenyl chloroformate, the temperature of the reaction solution was controlled not to exceed 40°C, the mixture was stirred at 30°C for 18 hours, the solvent was evaporated from the reaction mixture under reduced pressure at 40°C, and 50ml of water was slowly added to precipitate a solid. Stir for 30 minutes, filter, wait until the filter cake, wash the filter cake with a small amount of methanol, suction filter until there is no liquid dripping, remove the solid to dry, the dry solid is 7.8g, the yield is 90.1%, and the content is 98.3%.

example 3

[0006] Example 3 A 100ml flask is loaded with 5g (0.032mol) 2-amino-4,6-dimethoxypyrimidine, dissolved in 20ml ethyl acetate, added 6.4ml (0.048mol) N, N-dimethylaniline, slowly Add 6.4ml (0.048mol) phenyl chloroformate, control the temperature of the reaction solution not to exceed 40°C, stir the mixture at 30°C for 18 hours, evaporate the solvent from the reaction mixture at 40°C under reduced pressure, add 20ml of methanol to dissolve the solid , when there are no large solids, slowly add 30ml of water, precipitate crystals, stir for 30 minutes, filter, wait until the filter cake, wash the filter cake with a small amount of methanol, suction filter until there is no liquid dripping, remove the solid and dry it in the air The solid is 6.4g, the yield is 74.3%, and the content is 96.1%.

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PUM

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Abstract

The invention relates to a method for preparing 4, 6-dimethoxy-2(phenoxyl carboxide)amido)-pyrimidine) (DPAP for short). The method is characterized by comprising the following steps: adopting tetrahydrofuran, ethyl acetate or glycol dimethyl ether as a reaction solvent; with the ratio of grams of the reaction to reaction initiator 2-amido-4, 6-dimethoxy pyrimidine of between 2 to 1 and 10 to 1, in the presence of N, N-dimethylaniline with the molar weight of between 1.1 and 1.5, preparing the DPAP by a method of leading the 2-amido-4, 6-dimethoxy pyrimidine with 1 molar weight to react with benzyl chloroformate with molar weight of between 1.1 and 1.5 at normal pressure and at a temperature of between 20 and 40 DEG C; distilling solvent after the reaction; then adding water to the solvent to separate out a product; or dissolving the reaction mixture of the distilled solvent by methanol, and adding water with 1 to 5 times amount of the methanol to separate out the product; and washingthe crude product by 1 time amount of the methanol to obtain the product. The method has the advantages that the average purity of the product is higher than the average yield; and the used solvent can be reclaimed, thereby not only saving production cost, but also reducing discharge of waste water.

Description

technical field [0001] The invention relates to a preparation method of 4,6-dimethoxy-2-((phenoxycarbonyl)amino)-pyrimidine for short DPAP, and DPAP is an important intermediate for preparing sulfonylurea herbicide rimsulfuron-methyl. Because the purity of DPAP directly affects the purity and quality of its downstream preparation of the sulfonylurea herbicide rimsulfuron-methyl, the preparation technology of high-purity DPAP is the first step to produce qualified or high-purity sulfonylurea herbicide rimsulfuron-methyl. one of the key technologies. Background technique [0002] The Chinese patents CN 1178526A and CN 1089339C of U.S. Namur DuPont Company have taken in the inert solvent of 1,4-dioxane and tetramethylurea, in the presence of N,N-dimethylaniline, at 10 to DPAP was prepared by reacting 2-amino-4,6-dimethoxypyrimidine with phenyl chloroformate at a temperature of 45°C. The average purity of the final product obtained by this method is 97.1%, and the average yiel...

Claims

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Application Information

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IPC IPC(8): C07D239/52
Inventor 胡昆高学明宋国强蒋军任杰
Owner JIANGSU POLYTECHNIC UNIVERSITY
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