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Synthesizing method for 2,2-difluoro-1,3-benzodioxole

A synthesis method and a benzo-based technology are applied in the field of compound synthesis, which can solve the problems of long synthesis route and many kinds of raw materials, and achieve the effects of less process waste, simple process and high yield.

Inactive Publication Date: 2016-01-13
JIANGSU REPONT PESTICIDE FACTORY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

A synthetic route in the prior art is to generate sodium salt by reacting catechol and sodium hydroxide, react with dichloromethane under pressure to generate piperonyl ring, piperonyl ring is chlorinated, and react with hydrofluoric acid to generate 2 , 2-difluoro-1,3-benzodioxol, due to the long synthetic route and the variety of raw materials involved, so far, there is still a lack of 2,2-difluoro-1, which has simple steps and high yields. The synthetic method of 3-benzodioxol

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0008] (1) Put 370Kg of water into the reaction kettle, start stirring and add 163.3Kg of 98wt% sodium hydroxide, then add 20Kg of liquid paraffin, raise the temperature to control the temperature of the reaction kettle at 85°C, add catechol 220Kg, and keep the reaction The temperature of the kettle is 85°C. After the feeding is completed, react for 1 hour to obtain catechol sodium salt; (2) add 60Kg of water, 500Kg of toluene, and 40Kg of tetrabutylammonium sulfate to the autoclave, close the autoclave, and use nitrogen gas to Substitute three times, raise the temperature and control the temperature of the autoclave at 95°C, inject catechol sodium salt and dichlorodifluoromethane into the autoclave with a metering pump, and the catechol sodium salt needs to be preheated to 85~90℃, the feed rate of catechol sodium salt is 2.5Kg / min, the feed rate of dichlorodifluoromethane is 0.84Kg / min, the total feed rate of dichlorodifluoromethane is 252Kg, keep the autoclave temperature At...

Embodiment 2

[0010] (1) Put 440Kg of water in the reactor, start stirring and add 196Kg of 98wt% sodium hydroxide, then add 24Kg of liquid paraffin, heat up to control the temperature of the reactor at 85°C, add catechol 240Kg, keep the reactor The temperature is 85°C, after the feed is finished, react for 1 hour to obtain catechol sodium salt; (2) Add 72Kg of water, 600Kg of toluene, and 48Kg of tetrabutylammonium sulfate into the autoclave, close the autoclave, and replace with nitrogen Three times, the temperature was raised to control the temperature of the autoclave at 95°C, and the catechol sodium salt and dichlorodifluoromethane were injected into the autoclave with a metering pump, and the catechol sodium salt needed to be preheated to 85°C in advance. ~90°C, the feeding rate of catechol sodium salt is 2.5Kg / min, the feeding rate of dichlorodifluoromethane is 0.84Kg / min, and the total feeding rate of dichlorodifluoromethane is 302Kg, keep the autoclave temperature at 95~105°C, afte...

Embodiment 3

[0012] (1) Put 560Kg of water in the reactor, start stirring and add 245Kg of 98wt% sodium hydroxide, then add 30Kg of liquid paraffin, heat up to control the temperature of the reactor at 85°C, add catechol 330Kg, keep the reactor The temperature is 85°C, after the feed is finished, react for 1 hour to obtain catechol sodium salt; (2) Add 90Kg of water, 750Kg of toluene, and 60Kg of tetrabutylammonium sulfate into the autoclave, close the autoclave, and replace with nitrogen Three times, the temperature was raised to control the temperature of the autoclave at 95°C, and the catechol sodium salt and dichlorodifluoromethane were injected into the autoclave with a metering pump, and the catechol sodium salt needed to be preheated to 85°C in advance. ~90°C, the feeding rate of catechol sodium salt is 2.5Kg / min, the feeding rate of dichlorodifluoromethane is 0.84Kg / min, and the total feeding rate of dichlorodifluoromethane is 378Kg, keep the autoclave temperature at 95~105°C, afte...

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Abstract

The invention relates to a synthesizing method for 2,2-difluoro-1,3-benzodioxole. The method comprises the steps that 1, sodium hydroxide and water are added into a reaction kettle, then liquid paraffin is added, the temperature is increased to control the temperature of the reaction kettle to be under the condition of 85 DEG C, pyrocatechol is added, the temperature is kept at 85 DEG C, reacting is performed for 1 hour, and then pyrocatechol sodium salt is prepared; 2, methylbenzene, water and catalysts are added in a high-pressure kettle, the high-pressure kettle is closed, replacement is performed for three times with nitrogen, the temperature is increased to control the temperature of the high-pressure kettle to be under the condition of 95 DEG C, the pyrocatechol sodium salt prepared in the step 1 and dichlorodifluoromethane are added, the pyrocatechol sodium salt is preheated to 85 DEG C-90 DEG C in advance before being fed, the temperature of the high-pressure kettle is kept at 95 DEG C-105 DEG C, reacting is performed for 1 hour, the high-pressure kettle is cooled to 20 DEG C, an organic layer solution is separated out, washing is performed for one time, the organic layer solution is rectified to collect rectified components, and the 2,2-difluoro-1,3-benzodioxole is obtained. The synthesizing method for the 2,2-difluoro-1,3-benzodioxole has the advantages of being simple and direct in technology, few in technology waste materials, high in yield and suitable for large-scale industrialized production.

Description

technical field [0001] The invention relates to a compound synthesis method, in particular to a synthesis method of 2,2-difluoro-1,3-benzodioxol. Background technique [0002] 2,2-Difluoro-1,3-benzodioxol is used as an intermediate of medicine and pesticide. A synthetic route in the prior art is to generate sodium salt by reacting catechol and sodium hydroxide, react with dichloromethane under pressure to generate piperonyl ring, piperonyl ring is chlorinated, and react with hydrofluoric acid to generate 2 , 2-difluoro-1,3-benzodioxol, due to the long synthetic route and many types of raw materials involved, so far, there is still a lack of 2,2-difluoro-1, which has simple steps and high yields. Synthetic method of 3-benzodioxol. Contents of the invention [0003] The technical problem to be solved in the present invention is to provide a kind of synthetic method that can prepare 2,2-difluoro-1,3-benzodioxol with simple process and high yield, and its innovative point is...

Claims

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Application Information

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IPC IPC(8): C07D317/46
CPCC07D317/46
Inventor 步康明陈学彬徐海元胡俊
Owner JIANGSU REPONT PESTICIDE FACTORY
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