Method for synthesizing 3-(butoxy methyl phosphoryl)-1-cyanopropyl acetate based on micro-channel reactor

A cyanopropyl acetate and micro-channel reactor technology is applied in the field of glufosinate-ammonium intermediate synthesis, and can solve the problems of difficult control, high safety risk, low production efficiency and the like

Inactive Publication Date: 2020-12-22
SICHUAN FOURSTAR BIOTECH RANDD CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The present invention mainly aims at the synthesis method of 3-(butoxymethylphosphoryl)-1-cyanopropyl acetate intermediate in the existing glyphosate synthesis, which has many types of production equipment, high s

Method used

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  • Method for synthesizing 3-(butoxy methyl phosphoryl)-1-cyanopropyl acetate based on micro-channel reactor
  • Method for synthesizing 3-(butoxy methyl phosphoryl)-1-cyanopropyl acetate based on micro-channel reactor
  • Method for synthesizing 3-(butoxy methyl phosphoryl)-1-cyanopropyl acetate based on micro-channel reactor

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Embodiment 1

[0027] A method for synthesizing 3-(butoxymethylphosphoryl)-1-cyanopropyl acetate based on a microchannel reactor, comprising the following steps:

[0028] A. Turn on the heating system and light system (light wavelength 10nm) of the microchannel reactor to raise the temperature of the system to a reaction temperature of 30°C;

[0029] B. Metering monobutyl methylphosphinate and 1-cyano-2-propenyl acetate into the microchannel reactor (wherein, monobutyl methylphosphinate 3mol / min, 1-cyano- 2-propenyl acetate 1mol / min), the reaction pressure is normal pressure;

[0030] C. The two materials introduced in step B stay and react in the microchannel reactor for 0.5min. After the temperature reaches 120°C under 10mmHg pressure and stop distillation to remove low boilers, 3-(butoxymethylphosphoryl )-1-cyanopropyl acetate target product 3939.1g, gas chromatography detection 3-(butoxymethylphosphoryl)-1-cyanopropyl acetate content 96.9%, yield 97.4%.

Embodiment 2

[0032] A method for synthesizing 3-(butoxymethylphosphoryl)-1-cyanopropyl acetate based on a microchannel reactor, comprising the following steps:

[0033] A. Turn on the heating system and light system (light wavelength 700nm) of the microchannel reactor to raise the temperature of the system to a reaction temperature of 70°C;

[0034] B. Metering monobutyl methylphosphinate and 1-cyano-2-propenyl acetate into the microchannel reactor (wherein, monobutyl methylphosphinate 2mol / min, 1-cyano- 2-propenyl acetate 1mol / min), the reaction pressure is 1.8MPa;

[0035] C. The two materials introduced in step B stay and react in the microchannel reactor for 5 minutes. After the temperature reaches 125°C under the pressure of 10mmHg, the distillation is stopped to remove low boilers, and 3-(butoxymethylphosphoryl) is obtained. - 1-cyanopropyl acetate The target product was 3939g, the content of 3-(butoxymethylphosphoryl)-1-cyanopropyl acetate was 97.6% as detected by gas chromatograph...

Embodiment 3

[0037] A method for synthesizing 3-(butoxymethylphosphoryl)-1-cyanopropyl acetate based on a microchannel reactor, comprising the following steps:

[0038] A. Turn on the heating system and illumination system (light wavelength 100nm) of the microchannel reactor to heat up the system to a reaction temperature of 50°C;

[0039] B. Metering monobutyl methylphosphinate and 1-cyano-2-propenyl acetate into the microchannel reactor (wherein, monobutyl methylphosphinate 1.5mol / min, 1-cyano -2-propenyl acetate 1mol / min), the reaction pressure is 1MPa;

[0040] C. The two materials introduced in step B stay and react in the microchannel reactor for 2 minutes. After the temperature reaches 121°C under 10mmHg pressure and stop distillation to remove low boilers, 3-(butoxymethylphosphoryl) is obtained. - 1-cyanopropyl acetate The target product was 3937.9g, the content of 3-(butoxymethylphosphoryl)-1-cyanopropyl acetate was 97.3% as detected by gas chromatography, and the yield was 97.4%...

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Abstract

The invention relates to the technical field of glufosinate-ammonium intermediate synthesis, and particularly discloses a method for synthesizing 3-(butoxy methyl phosphoryl)-1-cyanopropyl acetate based on a micro-channel reactor, and mainly aims to solve the problems of various production equipment types, high safety risk, difficulty in control, low production efficiency and the like of the method for synthesizing 3-(butoxy methyl phosphoryl)-1-cyanopropyl acetate in the existing glyphosate synthesis method. Methyl phosphinic acid monobutyl ester and 1-cyano-2-allyl acetate is taken as raw materials, continuous reaction is carried out under photocatalysis, the excellent mass and heat transfer characteristics of the micro-channel reactor are utilized, and under the condition that the yieldcan reach 96% or above, the reaction period is greatly shortened, the safety risk is reduced, and the production efficiency is improved.

Description

technical field [0001] The invention relates to the technical field of synthesis of glufosinate-ammonium intermediates, in particular to a method for synthesizing 3-(butoxymethylphosphoryl)-1-cyanopropyl acetate based on a microchannel reactor. Background technique [0002] 3-(Butoxymethylphosphoryl)-1-cyanopropyl acetate is an intermediate in the synthesis of glufosinate-ammonium, and its molecular structure is as follows: [0003] , boiling point 175 ~ 180 ℃ (0.15mmHg). [0004] In the synthesis of glufosinate-ammonium, 3-(butoxymethylphosphoryl)-1-cyanopropyl acetate is generally catalyzed by a free radical initiator, from monobutyl methylphosphinate and 1-cyano Base-2-propenyl acetate is obtained by reacting at a certain temperature, and its synthetic reaction formula is as follows: [0005] [0006] In order to ensure the smooth progress of the reaction, this method uses an active free radical initiator to react for a long time at a lower temperature (about 4 hou...

Claims

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Application Information

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IPC IPC(8): C07F9/32B01J19/00
CPCC07F9/3211C07F9/3264B01J19/0093
Inventor 卢刚宋剑锋朱槽王长江
Owner SICHUAN FOURSTAR BIOTECH RANDD CORP
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