CN107513027A

CN107513027A - The production technology of Bifenazate

Info

Publication number: CN107513027A
Application number: CN201710764840.9A
Authority: CN
Inventors: 朱建永; 刘如成
Original assignee: Shanghai Kai Rong Chemical Technology Co Ltd
Current assignee: Shanghai Kai Rong Chemical Technology Co Ltd
Priority date: 2017-08-30
Filing date: 2017-08-30
Publication date: 2017-12-26

Abstract

A kind of production technology of Bifenazate, chosen, methylated by raw material, amination, Bifenazate synthesize these steps synthesis Bifenazate.The invention has the advantages that：Reactions steps are few, and production. art is simple and convenient, and production process is simple, eliminate cumbersome production stage, the reaction process time is short, it is possible to increase production efficiency, improves production economy benefit, and target compound high income, production yields can be improved, reduces production cost, using effect is good, beneficial to popularization.

Description

The production technology of Bifenazate

Technical field

The present invention relates to technical field of pesticide manufacture, more particularly to a kind of production technology of Bifenazate.

Background technology

At present, conventional Bifenazate production when, it is necessary to pass through nitrification, methoxylation, nitro reduce, diazotising reduction Reacted with amidatioon etc., synthesized purpose product Bifenazate, this conventional production method complex steps are complicated, reaction process Long, target compound yield is low, causes the production time among actual production process to grow, and productivity effect is low, and target product obtains Few, cost is high.

The content of the invention

The invention solves the above-mentioned problems of the prior art, there is provided a kind of production technology of Bifenazate, solves mesh Production process very complicated in preceding Bifenazate production process, the problem of target compound yield is low, meet that Bifenazate is given birth to The demand of production.

The present invention solves the technical scheme that its technical problem uses：The production technology of this Bifenazate, including following step Suddenly：

The first step, raw material are chosen, and choose parazon as the raw material for preparing Bifenazate；

Second step, methylate, 15kg~30kg pair is added into the retort of thermometer, agitator and reflux condensing tube Xenol, 2kg~6kg sulfate, 3kg~8kg ethyl methoxyacetates, 60L ethanol, are heated to 60 DEG C, 3kg are then added dropwise ~5kg dimethyl suflfate, time for adding about 3h, drop finish, and continue back flow reaction 5h, room temperature are cooled to, with 10kg~12kg salt It is 1~1.5 that water, which adjusts pH value, is subsequently poured into frozen water, has white solid precipitation, filtration drying, obtain white solid；

3rd step, amination, the addition 15kg~30kg white into the retort of thermometer, agitator and reflux condensing tube Solid, 3kg~5kg potassium hydroxide, 60L ethanol, 7kg~9kg hydrazines, 2h is reacted under the conditions of 50 DEG C, then with 10kg~12kg Concentrated hydrochloric acid regulation pH value is 1~1.5, now has gas effusion, when being produced without gas, reaction solution is cooled into room temperature, is had solid Body separates out, filtering, dry pale solid；

4th step, Bifenazate synthesis, into the retort of thermometer, agitator and reflux condensing tube add 15kg~ 30kg pale solid, 7kg~9kg alchlors, 60L water, 40 DEG C of reaction 6h~9h are warming up to, ethyl acetate extraction, are removed Water layer is removed, Bifenazate is obtained with 9kg~12kg re crystallization from toluene.

Further, 7.5h is reacted when being warming up to 40 DEG C in the 4th step.

The production technology of the Bifenazate of the present invention, the first step carry out raw material selection, and selection reaction effect is good, cost is low Parazon carries out methylation reaction as the raw material for preparing Bifenazate, second step, using ethyl methoxyacetate, reaction Greenization, safety and environmental protection, pollution being reduced, and improve target compound yield, the white solid of acquisition is 4- methoxyl biphenyls, 3rd step carries out amination, and pale solid is body N- (4- methoxyl biphenyl base -3- bases) diazanyl -1,2- dioctyl phthalate diisopropyl ester, 4th step synthesizes Bifenazate, and the yield of Bifenazate is improved using alchlor, improves product yield.

The invention has the advantages that：The present invention Bifenazate production technology, by methylating, amination, biphenyl hydrazine These steps of Lipase absobed can synthesize Bifenazate, and reactions steps are few, and production. art is simple and convenient, and production process is simple, eliminate Cumbersome production stage, reaction process time are short, it is possible to increase production efficiency, improve production economy benefit, and target chemical combination Thing high income, it is possible to increase production yields, reduce production cost, using effect is good, beneficial to popularization.

Embodiment

The invention will be further described below：

Embodiment one：

The production technology of this Bifenazate, comprises the following steps：

Second step, methylate, joining to hydroxyl for 15kg is added into the retort of thermometer, agitator and reflux condensing tube Benzene, 2kg sulfate, 3kg ethyl methoxyacetates, 60L ethanol, are heated to 60 DEG C, and 3kg dimethyl suflfate, drop is then added dropwise About 3h between added-time, drop finish, and continue back flow reaction 5h, are cooled to room temperature, and it is 1 to adjust pH value with 10kg salt solution, is subsequently poured into frozen water, There is white solid precipitation, filtration drying, obtain white solid；

3rd step, amination, into the retort of thermometer, agitator and reflux condensing tube add 15kg white solid, 3kg potassium hydroxide, 60L ethanol, 7kg hydrazines, 2h is reacted under the conditions of 50 DEG C, is then 1 with 10kg concentrated hydrochloric acids regulation pH value, this When have gas effusion, when being produced without gas, reaction solution is cooled to room temperature, there is solid precipitation, filter, it is dry that canescence is consolidated Body；

4th step, Bifenazate synthesis, the addition 15kg ash into the retort of thermometer, agitator and reflux condensing tube White solid, 7kg alchlors, 60L water, 40 DEG C of reaction 6h are warming up to, ethyl acetate extraction, water layer are removed, with 9kg toluene It is recrystallized to give Bifenazate.

Embodiment two：

The production technology of this Bifenazate, comprises the following steps：

Second step, methylate, joining to hydroxyl for 20kg is added into the retort of thermometer, agitator and reflux condensing tube Benzene, 4kg sulfate, 6kg ethyl methoxyacetates, 60L ethanol, are heated to 60 DEG C, and 4kg dimethyl suflfate, drop is then added dropwise About 3h between added-time, drop finish, and continue back flow reaction 5h, are cooled to room temperature, and it is 1.2 to adjust pH value with 11kg salt solution, is subsequently poured into frozen water In, there is white solid precipitation, filtration drying, obtain white solid；

3rd step, amination, into the retort of thermometer, agitator and reflux condensing tube add 20kg white solid, 4kg potassium hydroxide, 60L ethanol, 8kg hydrazines, 2h is reacted under the conditions of 50 DEG C, is then 1.2 with 11kg concentrated hydrochloric acids regulation pH value, Now there is gas effusion, when being produced without gas, reaction solution is cooled to room temperature, there is solid precipitation, filter, dry canescence Solid；

4th step, Bifenazate synthesis, the addition 20kg ash into the retort of thermometer, agitator and reflux condensing tube White solid, 8kg alchlors, 60L water, 40 DEG C of reaction 7.5h are warming up to, ethyl acetate extraction, water layer are removed, with 10kg's Re crystallization from toluene obtains Bifenazate.

Embodiment three：

The production technology of this Bifenazate, comprises the following steps：

Second step, methylate, joining to hydroxyl for 30kg is added into the retort of thermometer, agitator and reflux condensing tube Benzene, 6kg sulfate, 8kg ethyl methoxyacetates, 60L ethanol, are heated to 60 DEG C, and 5kg dimethyl suflfate, drop is then added dropwise About 3h between added-time, drop finish, and continue back flow reaction 5h, are cooled to room temperature, and it is 1.5 to adjust pH value with 12kg salt solution, is subsequently poured into frozen water In, there is white solid precipitation, filtration drying, obtain white solid；

3rd step, amination, into the retort of thermometer, agitator and reflux condensing tube add 30kg white solid, 5kg potassium hydroxide, 60L ethanol, 9kg hydrazines, 2h is reacted under the conditions of 50 DEG C, is then 1.5 with 12kg concentrated hydrochloric acids regulation pH value, Now there is gas effusion, when being produced without gas, reaction solution is cooled to room temperature, there is solid precipitation, filter, dry canescence Solid；

4th step, Bifenazate synthesis, the addition 30kg ash into the retort of thermometer, agitator and reflux condensing tube White solid, 9kg alchlors, 60L water, 40 DEG C of reaction 9h are warming up to, ethyl acetate extraction, water layer are removed, with 12kg first Benzene is recrystallized to give Bifenazate.

Choose the connection that Bifenazate prepared by the embodiment of the present invention one, embodiment two, embodiment three is prepared with conventional method Phenylhydrazine ester carries out content, yield contrast, and comparing result is as follows：

As can be known from the above table, the production technology of Bifenazate of the invention, the Bifenazate of acquisition are equal from content and yield Bifenazate prepared by excellent conventional method.

The characteristics of embodiment of the present invention is：By methylating, amination, Bifenazate synthesizes these steps can synthesize biphenyl Hydrazine ester, reactions steps are few, and production. art is simple and convenient, and production process is simple, eliminate cumbersome production stage, reaction process time It is short, it is possible to increase production efficiency, to improve production economy benefit, and target compound high income, it is possible to increase production yields, drop Low production cost, using effect is good, beneficial to popularization.

Although the present invention is described by reference to preferred embodiment, those skilled in the art should Work as understanding, in the range of claims, various change in form and details can be made.

Claims

1. a kind of production technology of Bifenazate, it is characterised in that comprise the following steps：

(1) raw material is chosen, and chooses parazon as the raw material for preparing Bifenazate；

(2) methylate, joining to hydroxyl for 15kg~30kg is added into the retort of thermometer, agitator and reflux condensing tube Benzene, 2kg~6kg sulfate, 3kg~8kg ethyl methoxyacetates, 60L ethanol, are heated to 60 DEG C, and 3kg~5kg is then added dropwise Dimethyl suflfate, time for adding about 3h, drop finish, continue back flow reaction 5h, be cooled to room temperature, with 10kg~12kg salt solution adjust pH It is worth for 1~1.5, is subsequently poured into frozen water, has white solid precipitation, filtration drying, obtain white solid；

(3) amination, 15kg~30kg white solid, 3kg are added into the retort of thermometer, agitator and reflux condensing tube ~5kg potassium hydroxide, 60L ethanol, 7kg~9kg hydrazines, react 2h under the conditions of 50 DEG C, are then adjusted with 10kg~12kg concentrated hydrochloric acids It is 1~1.5 to save pH value, now has gas effusion, when being produced without gas, reaction solution is cooled into room temperature, there is solid precipitation, mistake Filter, dry pale solid；

(4) Bifenazate is synthesized, and the greyish white of 15kg~30kg is added into the retort of thermometer, agitator and reflux condensing tube Color solid, 7kg~9kg alchlors, 60L water, 40 DEG C of reaction 6h~9h are warming up to, ethyl acetate extraction, water layer is removed, uses 9kg~12kg re crystallization from toluene obtains Bifenazate.

2. the production technology of Bifenazate according to claim 1, it is characterised in that：Heating heating in the step (3) 7.5h is reacted during to 40 DEG C.