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Method for continuously synthesizing 5 (2-ethylthio propyl)-2-propionyl-3-hydroxyl-2-cyclohexene-1 ketone by using micro-channel reactor

A technology of microchannel reactor and ethylthiopropyl, which is applied in chemical instruments and methods, chemical/physical/physicochemical reactors, thioether preparation, etc., can solve the problem of high production cost, prone to side reactions, Low product content and other issues, to achieve the effects of no amplification effect, shortened production cycle, and high product yield

Inactive Publication Date: 2020-10-23
辽宁先达农业科学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In the prior art, in the preparation of 5-(2-ethylthiopropyl)-2-propionyl-3-hydroxyl-2-cyclohexen-1-one, because the acylated material is unstable by itself, Side reactions are prone to occur in subsequent reactions, resulting in low conversion rates, low product content, and high overall production costs

Method used

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  • Method for continuously synthesizing 5 (2-ethylthio propyl)-2-propionyl-3-hydroxyl-2-cyclohexene-1 ketone by using micro-channel reactor

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Embodiment 1

[0035] The continuous synthesis method of 5(2 ethylthiopropyl)-2 propionyl-3 hydroxy-2 cyclohexene-1 ketone in the microchannel reactor of this embodiment includes:

[0036] The microchannel reactor is a three-stage reactor, and the microchannel reactor includes the first microchannel reactor, the second microchannel reactor and the third microchannel reactor communicated in sequence, and the third microchannel reactor The outlet port of the microchannel reactor is connected with the pipe reactor; the specific synthesis using this microchannel reactor includes the following contents:

[0037] The toluene solution (mass concentration is 24%) of acylate (compound 1) and the toluene solution (mass concentration is 5.5%) of DMAP are passed in the first stage microchannel reactor, and the flow velocity of the toluene solution of compound 1 is 3mL / min, the toluene solution flow rate of DMAP is 0.4mL / min, stay 7min at 150 ℃, the reaction solution enters the second-stage microchannel...

Embodiment 2

[0039] The continuous synthesis method of 5(2 ethylthiopropyl)-2 propionyl-3 hydroxy-2 cyclohexene-1 ketone in the microchannel reactor of this embodiment includes:

[0040] The microchannel reactor is a three-stage reactor, and the microchannel reactor includes the first microchannel reactor, the second microchannel reactor and the third microchannel reactor communicated in sequence, and the third microchannel reactor The outlet port of the microchannel reactor is connected with the pipe reactor; the specific synthesis using this microchannel reactor includes the following contents:

[0041]The toluene solution (mass concentration is 24%) of acylate (compound 1) and the toluene solution (mass concentration is 5.5%) of DMAP are passed in the first stage microchannel reactor, and the flow velocity of the toluene solution of compound 1 is 6mL / min, the toluene solution flow rate of DMAP is 0.8mL / min, stay at 160 ℃ for 3.5min, the reaction solution enters the second-stage microch...

Embodiment 3

[0043] The continuous synthesis method of 5(2 ethylthiopropyl)-2 propionyl-3 hydroxy-2 cyclohexene-1 ketone in the microchannel reactor of this embodiment includes:

[0044] The microchannel reactor is a three-stage reactor, and the microchannel reactor includes the first microchannel reactor, the second microchannel reactor and the third microchannel reactor communicated in sequence, and the third microchannel reactor The outlet port of the microchannel reactor is connected with the pipe reactor; the specific synthesis using this microchannel reactor includes the following contents:

[0045] The toluene solution (mass concentration is 24%) of acylate (compound 1) and the toluene solution (mass concentration is 5.5%) of DMAP are passed in the first stage microchannel reactor, and the flow velocity of the toluene solution of compound 1 is 6mL / Min, the toluene solution flow rate of DMAP is 0.8mL / min, stay 3.5min at 160 ℃, the reaction solution enters the second-stage microchann...

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Abstract

The invention relates to a method for continuously synthesizing 5 (2-ethylthio propyl)-2-propionyl-3-hydroxyl-2-cyclohexene-1 ketone by using a micro-channel reactor. The method comprises the following steps: introducing a toluene solution of a compound 1 and a toluene solution of DMAP into a first micro-channel reactor to perform translocation reaction; and introducing the compound 2 and a sodiumhydroxide solution into a second micro-channel reactor, carrying out a hydrolysis reaction to obtain a compound 3, introducing the compound 3 and a hydrochloric acid solution into a third micro-channel reactor, carrying out a neutralization decarboxylation reaction, introducing the reaction solution into a pipeline reactor, cooling, and desolventizing to obtain the product. Compared with an existing production process adopting a conventional reaction kettle, the heat and mass transfer process is uniform, the amplification effect is avoided, side reactions can be effectively reduced, and thusthe conversion rate of raw materials is increased. According to the method, the reaction time is greatly shortened, continuous production can be realized, the production efficiency is improved, and the production cost is reduced.

Description

technical field [0001] The invention belongs to the field of synthesis of herbicide clethodim intermediate, in particular to a microchannel reactor for continuous synthesis of 5-(2-ethylthiopropyl)-2-propionyl-3-hydroxy-2-cyclohexene -1-one method. Background technique [0002] Weeds in farmland are one of the main problems to be solved in agricultural production. Cyclohexenone herbicide clethodim has special effects on most annual and perennial grass weeds. As an important intermediate of clethodim, 5-(2-ethylthiopropyl)-2-propionyl-3-hydroxy-2-cyclohexen-1-one has been widely used. [0003] At present, the commonly used preparation method of 5-(2-ethylthiopropyl)-2-propionyl-3-hydroxyl-2-cyclohexen-1-one utilizes 6-ethylthio-3-heptene-2 - Ketone and propionyl chloride are the main raw materials, after acylation, rearrangement, hydrolysis, and then extraction and desolventization to obtain 5-(2-ethylthiopropyl)-2-propionyl-3-hydroxy-2-cyclohexyl en-1-one. [0004] In th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C319/20C07C323/55B01J19/00
CPCC07C319/20B01J19/0093C07C323/55
Inventor 郑志明邢静李凯李大为刘泉民张辉李莉李磊磊董培闫永军成功李志华强国英邹亚波任八玉彭军
Owner 辽宁先达农业科学有限公司