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Preparation method of substituted diphenyl ether bromide

A kind of technology of bromide, diphenyl ether

Pending Publication Date: 2020-08-25
QINGDAO KYX CHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention aims at problems such as low selectivity, long reaction time, and non-continuous production caused by poor mass and heat transfer of traditional equipment in the bromination process of substituted diphenyl ether compounds, and proposes a modular reaction device using microchannels The method for brominating the substituted diphenyl ether compound enables the substituted diphenyl ether compound and liquid bromine to complete the bromination reaction of the hydrogen atom on the methyl position with high selectivity under the conditions of fast and efficient mixing, and its main advantages are It can realize continuous production, and at the same time achieve the purpose of reducing energy consumption, simplifying production process, improving production efficiency and reaction safety

Method used

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  • Preparation method of substituted diphenyl ether bromide
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  • Preparation method of substituted diphenyl ether bromide

Examples

Experimental program
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Effect test

Embodiment 1

[0044] A kind of preparation method of the bromide of substituted diphenyl ether, concrete steps are as follows:

[0045] 0.070mol of 2-methyl-2-[2-chloro-4-(4-chlorophenoxy)phenyl]-4-methyl-1,3-dioxolane (23.7g) was dissolved in 23.7 g cyclohexane, after mixing, add in the raw material bottle 1, add 11.5g cyclohexane in the 0.072mol liquid bromine (11.5g) and add in the raw material bottle 2 after mixing, open the temperature control system, make the microchannel reactor The temperature of the solution is 30°C. Preheat the cyclohexane solution of the cyclic compound in the raw material bottle 1 to 20-25°C with a flow pump, and enter the microreactor at a flow rate of 1ml / min. At the same time, the bromine solution in the raw material bottle 2 The cyclohexane solution is preheated to 20-25°C in advance, and enters the microreactor at a flow rate of 1.8ml / min. Through the temperature control system, the two react in the microreactor at 25-30°C. Sampling is analyzed by liquid c...

Embodiment 2

[0047] A kind of preparation method of the bromide of substituted diphenyl ether, concrete steps are as follows:

[0048] Dissolve 1mol of 2-methyl-2-[2-chloro-4-(4-chlorophenoxy)phenyl]-4-methyl-1,3-dioxolane (338.05g) in 338.05g In cyclohexane, add in raw material bottle 1 after mixing, add 164.6g cyclohexane in 1.03mol liquid bromine (164.6g) and add in raw material bottle 2 after mixing, open temperature control system, make the microchannel reactor The temperature is 30°C. Preheat the cyclohexane solution of the cyclic compound in the raw material bottle 1 to 20-25°C with a flow pump, and enter the microreactor at a flow rate of 3.5ml / min. At the same time, the bromine solution in the raw material bottle 2 is The cyclohexane solution is preheated to 20-25°C in advance, and enters the microreactor at a flow rate of 1.2ml / min. Through the temperature control system, the two react in the microreactor at 25-30°C. Sampling is analyzed by liquid chromatography. After the react...

Embodiment 3

[0050] A kind of preparation method of the bromide of substituted diphenyl ether, concrete steps are as follows:

[0051] Dissolve 2mol of 2-methyl-2-[2-chloro-4-(4-methylphenoxy)phenyl]-4-n-propyl-1,3-dioxolane (695g) in 700g In cyclohexane, add in raw material bottle 1 after mixing, add 321.6g cyclohexane in 2.01mol liquid bromine (321.6g) and add in raw material bottle 2 after mixing, open temperature control system, make the microchannel reactor The temperature is 30°C. Preheat the cyclohexane solution of the cyclic compound in the raw material bottle 1 to 20-25°C with a flow pump, and enter the microreactor at a flow rate of 4.0ml / min. At the same time, the bromine solution in the raw material bottle 2 is The cyclohexane solution is preheated to 20-25°C in advance, and enters the microreactor at a flow rate of 1.3ml / min. Through the temperature control system, the two react in the microreactor at 25-30°C. Sampling is analyzed by liquid chromatography. After the reaction ...

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Abstract

The invention relates to a preparation method of a substituted diphenyl ether bromide, which comprises the following steps: adding a substituted diphenyl ether compound and bromine into a micro-reactor, and carrying out continuous reaction to prepare the diphenyl ether compound of which the methyl hydrogen atom is substituted by bromine. According to the technical scheme, a modular micro-channel reaction device is adopted, so that the mass transfer and heat transfer efficiency is high, raw materials are instantly and fully mixed, the reaction rate is increased, the selectivity is improved, thereaction time is greatly shortened, and the production efficiency is improved; continuous production operation can be achieved, the product quality stability is improved, the equipment integration degree is high, and the occupied space can be reduced; and the product is high in yield and purity.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a preparation method of a substituted diphenyl ether bromide. Background technique [0002] Diphenyl ether compounds are now common pesticide compounds. Due to their unique physical and chemical properties and biological activities, they have been widely used in pesticide research in recent years, especially in the creation of new pesticides. Those containing diphenyl ether structures have biological activity. Compounds continue to emerge. The introduction of diphenyl ether structures into pesticide compounds can significantly improve the physical and chemical properties and biological activities of pesticides, such as increasing biological activity, expanding the control spectrum, and reducing toxicity to mammals. At present, the widely used insecticidal active compounds with diphenyl ether structure include phenothrin, fenoxycarb, methoprene, etc., and th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/22C07B39/00
CPCC07D317/22C07B39/00
Inventor 葛家成王旭栾明奎毕旌富矫立鹏王良清
Owner QINGDAO KYX CHEMICAL CO LTD
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