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Production method of metamitron

A technology of promethazone and its production method, which is applied in the field of herbicide preparation, and can solve the problems of high price of phase transfer catalyst, increased cost, large amount of water-absorbing agent, etc.

Inactive Publication Date: 2016-12-07
南通泰仓化学新材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The deficiency of above-mentioned two kinds of methods all is: (1) yield is lower, less than 90%
(2) The amount of water-absorbing agent is large (excessive water-absorbing agent), which increases the cost
The deficiency of this method is: the price of phase transfer catalyst is higher, and sodium benzoate is also higher relative to sodium acetate price, thereby causes production cost higher

Method used

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  • Production method of metamitron
  • Production method of metamitron
  • Production method of metamitron

Examples

Experimental program
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Embodiment Construction

[0034] 1. Hydrolysis and esterification

[0035] At normal temperature, pump the measured water into the hydrolysis kettle, put in the weighed benzoyl cyanide and stir and mix, slowly add concentrated sulfuric acid from the metering tank to the kettle under the stirring condition, and the kettle jacket is passed through the cooling water to control the temperature of the kettle. The internal temperature does not exceed 40°C. After the dropwise addition, stir and react for 2 hours, then put the measured hydrochloric acid (a small amount) into the kettle and stir, and control it at 45°C. After the completion, the jacket was heated to 60°C for 4 hours of heat preservation reaction; after the reaction was completed, the jacket was cooled to normal temperature, a certain amount of trichlorethylene was put into the kettle to stir for extraction, the layers were left to stand, and the lower water phase was released to the collection tank. The organic phase is transferred to the organ...

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Abstract

The invention discloses a production method of metamitron. The production method is characterized by comprising the following steps that benzoyl cyanide is hydrolyzed under the condition of H2SO4, and is then alcoholized into ester; hydrazine hydrate and methyl acetate take reaction to generate acetyl hydrazine hydrate; methyl benzoylformate and the acetyl hydrazine hydrate take reaction to generate hydrazine hydrate ester under the condition of H2SO4; hydrazine hydrate ester suspension and hydrazine hydrate take reaction; acyl is subjected to hydrazine treatment again to generate benzoyl hydrazine, and byproducts of methyl alcohol and water are generated; the benzoyl hydrazine is subjected to distillation, backflow, dehydration, cyclization and crystallization under the condition with a butanol solvent and a catalyst to generate the metamitron. The production method has the advantages that the cost of phase transfer catalysts is low; the cost of sodium benzoate is lower than that of sodium acetate, so that the production cost is reduced.

Description

technical field [0001] The invention relates to a preparation method of a herbicide, in particular to a preparation method of fenmetrione. Background technique [0002] The chemical name of metamitron is 4-amino-3-methyl-6-phenyl-1,2,4-triazin-5(4H)-one. It is a low-toxicity and low-residue herbicide developed by Bayer in 1975. It is a triazone selective pre-emergent herbicide. It is mainly absorbed through the roots of plants and then transported into the leaves. Er reaction to play a herbicidal effect. It can control monocotyledonous and dicotyledonous weeds. It is a herbicide used to control gramineous and broad-leaved weeds in beet fields. It is mainly used for field weeding of dryland crops, such as corn and sugar beets. Straw, wild sesame, bluegrass and other weeds. At present, the main route of synthesizing benzoylformate is as follows: first, methyl benzoylformate and acetylhydrazide are reacted to obtain 2-acetylhydrazinobenzoylformate, and then 2-acetylhydrazino...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D253/07
Inventor 鲍菊篱鲍明路
Owner 南通泰仓化学新材料有限公司
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