Process for preparing 3,4-dimethylpyrazole phosphate

A technology of dimethylpyrazole phosphate and dimethylpyrazole, which is applied in 3 fields, can solve the problems of long reaction time and achieve the effects of short reaction time, less by-products and mild reaction conditions

Inactive Publication Date: 2012-07-11
AVIC FERTILIZER
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Problems solved by technology

Although the two-step reaction of this scheme is carried out at room temperature, the reaction conditions are relatively mild, but the reaction time is relatively long, requiring 16-24 hours, and there will be isomers in the process of strong base catalysis to generate intermediate products, and there will be by-products in the end 3-Ethylpyrazole formation

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  • Process for preparing 3,4-dimethylpyrazole phosphate
  • Process for preparing 3,4-dimethylpyrazole phosphate
  • Process for preparing 3,4-dimethylpyrazole phosphate

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[0025] The invention provides a method for preparing 3,4-dimethylpyrazole phosphate. In the method, an organic solvent of sodium metal is used to replace a strong base, so that 2-butanone and ethyl formate undergo a condensation reaction to generate 2- Sodium methyl-3-oxobutyraldehyde, so as to synthesize 3,4-dimethylpyrazole with high selectivity. The reaction of 3,4-dimethylpyrazole with phosphoric acid gives 3,4-dimethylpyrazole phosphate.

[0026] The invention provides a method for effectively synthesizing 3,4-dimethylpyrazole phosphate with readily available raw materials, mild reaction conditions, short reaction time and few by-products.

[0027] see figure 1 , figure 1 It is a flowchart of the preparation method of 3,4-dimethylpyrazole phosphate of the present invention, and the preparation method of 3,4-dimethylpyrazole phosphate comprises: step S1, mixing metal sodium with 2-butanone and formic acid The mixed solution of ethyl ester generates sodium 2-methyl-3-oxo...

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Abstract

The invention provides a process for preparing 3,4-dimethylpyrazole phosphate, which includes the steps: (1) reacting metallic sodium with 2-butanone and ethyl formate to produce 2-methyl-3-oxobutanoic acid sodium salt; (2) reacting hydrazine hydrate with the 2-methyl-3-oxobutanoic acid sodium salt to produce 3,4-dimethyl pyrazole; and (3) reacting the 3,4-dimethyl pyrazole with phosphoric acid to produce the 3,4-dimethylpyrazole phosphate. The process for preparing the 3,4-dimethylpyrazole phosphate has the advantages that raw materials are easy to obtain, reaction conditions are mild, the reaction time is short and by-products are few.

Description

technical field [0001] The present invention relates to a preparation method of 3,4-dimethylpyrazole phosphate, in particular to a preparation method capable of efficiently synthesizing 3,4-dimethylpyrazole phosphate Background technique [0002] In various agricultural production activities, people use a large amount of chemical fertilizers unreasonably in pursuit of crop yields. According to surveys, the current average annual amount of pure nitrogen in my country is 200kg / ha. In economically developed areas such as the Taihu Lake Basin, the annual amount of pure nitrogen applied reaches more than 600kg / ha, and in many areas, the amount of pure nitrogen used is even as high as 500-1300kg / ha. Nitrogen fertilizers are easily lost after application. In addition, the scope of agricultural activities is huge, and the non-point source pollution produced is far away. Much larger impact than industrial point source pollution. According to a survey, the total nitrogen loss rate of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D231/12
Inventor 卢然郭长青张肖飞马杰文刘兴斌张浩军马宾曹明慧
Owner AVIC FERTILIZER
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