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Synthetic method of 2-hydroxyl-4,6-dimethyl pyrimidine hydrochloride

A technology of dimethylpyrimidine hydrochloride and a synthesis method, applied in directions such as organic chemistry, can solve problems such as being unfavorable for recycling, polluting the environment, increasing costs, etc., and achieves solvent recycling, less environmental pollution, and low cost. Effect

Active Publication Date: 2013-05-01
JINGBO AGROCHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the selection of ethanol as solvent, the method has the disadvantages of easy volatilization during recovery and miscibility with water, which is not conducive to recovery and reuse and increases the cost; ether is used for post-treatment, which has the disadvantages of polluting the environment, cumbersome operation, low yield and high cost shortcoming

Method used

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  • Synthetic method of 2-hydroxyl-4,6-dimethyl pyrimidine hydrochloride
  • Synthetic method of 2-hydroxyl-4,6-dimethyl pyrimidine hydrochloride
  • Synthetic method of 2-hydroxyl-4,6-dimethyl pyrimidine hydrochloride

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Experimental program
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Effect test

Embodiment 1

[0024] In a 250ml four-neck flask, add acetylacetone 52g, urea 60g, ethyl acetate 250ml, hydrochloric acid (36%) 100ml, heat reaction for 5 hours, HPLC is followed, the characteristic peak of acetylacetone disappears, indicating that the reaction is over; Add 250ml of methanol to the ester and water, filter, and dry to obtain the product. The product quality is 80.5g, the content is 97.1%, and the yield is 97.3%.

Embodiment 2

[0026] In a 250ml four-neck flask, add acetylacetone 52g, urea 48g, methylene chloride 200ml, hydrochloric acid (36%) 125ml, heat reaction for 6 hours, follow by HPLC, the disappearance of the characteristic peak of acetylacetone indicates the end of the reaction; Add 200ml of methanol to methane and water, filter, and dry to obtain the product. The product quality is 79.9g, the content is 97.6%, and the yield is 97.1%.

Embodiment 3

[0028] In a 250ml four-neck flask, add acetylacetone 52g, urea 36g, dichloroethane 150ml, hydrochloric acid (36%) 156ml, heat reaction for 8 hours, HPLC is followed, the disappearance of the characteristic peak of acetylacetone indicates that the reaction is over; Ethyl chloride and water, add 150ml of methanol, filter, dry to obtain the product, the product quality is 79.1g, the content is 98.7%, and the yield is 97.2%.

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Abstract

The invention relates to the technical field of chemical industries, in particular to a synthetic method of 2-hydroxyl-4,6-dimethyl pyrimidine hydrochloride. According to the method, as acetyl acetone and carbamide serve as reactants, an organic solvent which is not soluble in water serves as a reaction system solvent, 2-hydroxyl-4,6-dimethyl pyrimidine hydrochloride can be prepared in an efficient and environment-friendly; with the adoption of the method, the reaction speed is increased; the product quality is improved; a product yield is increased; and the method has the advantages that the yield is high, the environmental pollution is low, the solvent can be recycled, and the cost is low.

Description

technical field [0001] The invention relates to the technical field of petrochemical industry, and relates to a synthesis technology of a pesticide intermediate, in particular to a synthesis method of pyrimethanil intermediate 2-hydroxyl-4,6-dimethylpyrimidine hydrochloride. Background technique [0002] The English name of pyrimethanil is Pyrimethanil, and its chemical name is N-(4,6-dimethylpyrimidin-2-yl)aniline (4,6-dimethyl-N-phenyl-2-pyrimidinamine). The appearance of the product is white crystal. [0003] Pyrimethanil is a phenylpyrimidinamine fungicide with a unique mechanism of action. The drug mainly inhibits the secretion of proteins by pathogens, reduces the content of certain hydrolytic enzymes, and then penetrates into the host tissue to cause necrosis. It is the same as triazoles, morpholines, dicarboximides, and thiocarbamic acid Esters, benzimidazoles, phenylpyrroles, and Ditofencarb have no cross-resistance, have special effects on sensitive and resistant...

Claims

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Application Information

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IPC IPC(8): C07D239/36
Inventor 邱蓓吴文雷李洪侠刘英贤栾波马韵升
Owner JINGBO AGROCHEM TECH CO LTD