Method for preparing emamectin benzoate intermediate by microreactor

A technology of microreactor and microchannel reactor, which is applied in chemical instruments and methods, preparation of sugar derivatives, sustainable manufacturing/processing, etc., can solve problems such as non-continuous production, long reaction time, and low selectivity, and achieve Increased production efficiency, high product yield, and high mass transfer efficiency

Pending Publication Date: 2019-12-31
SHANGDONG HAILIER CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] The present invention aims at the extremely rapid heat release in the C4"-position oxide synthesis process due to the poor mass and heat transfer of traditional equipment in the production process of emamectin benzoate intermediates, resulting in low selectivity, long reaction time, and inability to continue production. problem, a method for the preparation of this intermediate using a microchannel modular reaction device was proposed

Method used

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  • Method for preparing emamectin benzoate intermediate by microreactor
  • Method for preparing emamectin benzoate intermediate by microreactor
  • Method for preparing emamectin benzoate intermediate by microreactor

Examples

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Effect test

Embodiment 1

[0042] A kind of method utilizing microreactor to prepare emamectin benzoate intermediate, concrete steps are as follows:

[0043] 1) Dissolve Abamectin and Tetramethylethylenediamine in dichloromethane to form a homogeneous solution. The solution and allyl chloroformate are pumped into micro-reaction module A respectively to control Abamectin: Tetramethylethylenediamine The molar ratio of amine: dichloromethane: allyl chloroformate is 1:5:20:1.3, react at -15°C, and the residence time is 15s. Sampling and testing the reaction through the sampling valve, and compound Ⅰ is obtained after the reaction is completed ;

[0044] 2) The compound I reaction liquid flowing out in step (1) is mixed with the pumped dimethyl sulfoxide in the micro-mixer and then flows into the micro-reaction module B, where it reacts with the phenyl dichlorophosphate pumped in at the same time, and the control Abamectin: dimethyl sulfoxide: the molar ratio of phenyl dichlorophosphate is 1:2:1.3, the cont...

Embodiment 2

[0056] A kind of method utilizing microreactor to prepare emamectin benzoate intermediate, concrete steps are as follows:

[0057] 1) Dissolve Abamectin and Tetramethylethylenediamine in dichloromethane to form a homogeneous solution, and pump allyl chloroformate into micro-reaction module A at the same time to control Abamectin: Tetramethylethylenediamine The molar ratio of amine: dichloromethane: allyl chloroformate is 1:2.5:35:1.05, react at -10°C, and the residence time is 15s. Sampling and testing the reaction through the sampling valve, and compound Ⅰ is obtained after the reaction is completed ;

[0058] 2) The compound I reaction solution flowing out of step (1) is mixed with the pumped dimethyl sulfoxide in the micro-mixer and then flows into the micro-reaction module B, where it reacts with the phenyl dichlorophosphate pumped in at the same time. The molar ratio of vermectin: dimethyl sulfoxide: phenyl dichlorophosphate is 1:1.95:1.0, the reaction temperature is con...

Embodiment 3

[0070] A kind of method utilizing microreactor to prepare emamectin benzoate intermediate, concrete steps are as follows:

[0071] 1) Abamectin and tetramethylethylenediamine are dissolved in dichloromethane to form a homogeneous solution A, and solution A and allyl chloroformate are pumped into micro-reaction module A respectively to control the avermectin: tetramethyl The molar ratio of ethylenediamine: dichloromethane: allyl chloroformate is 1:3.5:35:1.07, react at a temperature of -15°C, and the residence time is 10s. Sampling and detection of the reaction is carried out through the sampling valve. After the reaction is completed, Compound I;

[0072] 2) The compound I reaction solution flowing out of step (1) is mixed with the pumped dimethyl sulfoxide in the micro-mixer and then flows into the micro-reaction module B, where it reacts with the phenyl dichlorophosphate pumped in at the same time. The molar ratio of vermectin: dimethyl sulfoxide: phenyl dichlorophosphate i...

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Abstract

The invention relates to a method for preparing an emamectin benzoate intermediate by a microreactor. In particular, the method comprises the following steps: dissolving abamectin and tetramethylethylenediamine into dichloromethane to form a homogeneous solution, pumping the homogeneous solution and allyl chloroformate into a microchannel modular reaction device respectively to generate a compoundI; after mixing the reaction liquid of the compound I and dimethyl sulfoxide, pumping the mixture and phenyl dichlorophosphate into the next modular microreactor respectively to obtain a compound II;adjusting the pH of the reaction to 6 to 8 by alkaline water, standing and separating out an organic phase; distilling the organic phase and removing the dichloromethane to obtain the emamectin benzoate intermediate 4''-surface-4''-carbonyl-5-allyl formate-abamectin B1. According to the technical scheme of the invention and by adoption of the microchannel reaction device, mass transfer efficiencyand heat transfer efficiency are high, the raw materials are mixed instantaneously and completely, the reaction rate is accelerated, the selectivity is improved, the reaction time is greatly shortened and the production efficiency is improved; continuous production operation can be conducted, product quality stability is improved, the equipment integration level is high and occupied space can bereduced; and the product has high yield and high purity.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a method for preparing an intermediate of emamectin benzoate using a microreactor. Background technique [0002] Emamectin benzoate, emamectin benzoate, is a low-toxicity, high-efficiency, green, bio-sourced insecticide, which solves the problems of high toxicity, resistance and environmental impact of traditional pesticides . Emamectin benzoate has incomparable activity against many pests, especially against Lepidoptera, Diptera and thrips on vegetables, cotton, rice, potatoes, tobacco and other crops. It is safe for crops and has no systemic properties, but it can effectively penetrate into the epidermal tissue of applied crops, so it has a long residual effect period and is rarely affected by environmental factors such as wind and rain; the drug is easy to degrade in soil, no pollution, no residue, It is safe to beneficial insects, natural enemies of pe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/08C07H1/00
CPCC07H17/08C07H1/00Y02P20/10
Inventor 葛家成姚明磊单长岭王旭李建国
Owner SHANGDONG HAILIER CHEM
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