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Method for high-pressure liquid-phase isomerized production of acephate

An acephate, high pressure liquid phase technology, applied in chemical instruments and methods, organic chemistry, compounds of Group 5/15 elements of the periodic table, etc., can solve the problem of large waste water discharge, easy decomposition of catalyst ammonium sulfide, and complicated operation. and other problems, to achieve the effect of reducing pollution, high yield and simple process

Inactive Publication Date: 2015-04-29
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the yield of this method is very high, the catalyst ammonium sulfide is easy to decompose, the discharge of wastewater in the process is large, and the operation is cumbersome (UP3832425)

Method used

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  • Method for high-pressure liquid-phase isomerized production of acephate

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Embodiment 1

[0020] Embodiment 1, a method for producing acephate by isomerization of acetylspermine under high pressure, using acetylspermine as raw material, the following steps are carried out successively:

[0021] (1) In the pressure vessel, add 1.83g (10mmol) acetylspermine and 71mg (0.5mmol) methyl iodide, in the air atmosphere, slowly compress the gas, thereby increasing the pressure of the vessel to 100Mpa, the reaction temperature is controlled at 50°C, Stop the reaction after shaking for 2 hours;

[0022] (2) Lower the temperature to room temperature, remove the pressure to normal pressure, open the pressure vessel, remove methyl iodide under reduced pressure, and reclaim acetylspermine (obtaining 0.09g acetylspermine) by distillation under reduced pressure to obtain the product acephate 1.74g (Yield 95.1%).

Embodiment 2

[0023] Embodiment 2, a method for producing acephate by isomerization of acetylspermine under high pressure, using acetylspermine as raw material, the following steps are carried out successively:

[0024] (1) In a pressure vessel, add 1.83g (10mmol) of acetylspermine and 71mg (0.5mmol) of methyl iodide, in an air atmosphere, slowly compress the gas, increase the pressure of the vessel to 150Mpa, control the reaction temperature at 60°C, and shake Stop reaction after reacting 6h;

[0025] (2) Lower the temperature to room temperature, remove the pressure to normal pressure, open the pressure vessel, remove methyl iodide under reduced pressure, and reclaim acetylspermine (obtaining 0.02g acetylspermine) by distillation under reduced pressure to obtain 1.81g of product acephate (Yield 98.9%).

Embodiment 3

[0026] Embodiment 3, a method for producing acephate by isomerization of acetylspermine under high pressure, using acetylspermine as raw material, the following steps are carried out in sequence:

[0027] (1) In a pressure vessel, add 1.83g (10mmol) acetylspermine and 71mg (0.5mmol) methyl iodide, in a nitrogen atmosphere, slowly compress the gas, increase the pressure of the vessel to 50Mpa, control the reaction temperature at 80°C, and shake Stop reaction after reacting 4h;

[0028] (2) Lower the temperature to room temperature, remove the pressure to normal pressure, open the pressure vessel, remove methyl iodide under reduced pressure, and reclaim acetylspermine (obtaining 0.27g acetylspermine) by distillation under reduced pressure to obtain 1.56g of product acephate (Yield 85.2%).

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Abstract

The invention discloses a method for high-pressure liquid-phase isomerized production of acephate. The method comprises the following steps: carrying out liquid-phase isomerized reaction on acetyl arginine and methyl iodide at 50-120 Mpa and 30-80 DEG C under an oscillation condition for 1-6 h, wherein the mole ratio of the methyl iodide to the acetyl arginine is 2-10%; decompressing the reaction product to remove the methyl iodide, and distilling the acetyl arginine at reduced pressure to obtain the acephate. The method for preparing the acephate has the technical advantages of being simple in process, simple in aftertreatment and high in yield.

Description

technical field [0001] The invention relates to a liquid-phase isomerization of O, O-dimethyl-N-acetylphosphorothioate (acetylspermine for short) under high pressure to convert it into O, S-dimethyl-N-acetyl The method of phosphamide (acephate). Background technique [0002] O,S-Dimethyl-N-acetylphosphamide, commonly known as acephate, is a systemic contact insecticide with high efficiency, low toxicity and low residue, which is used to control Lepidoptera, Hemiptera Pests such as Homoptera and Homoptera have remarkable efficacy, but the toxicity is only one-fiftieth of that of methamidophos. Therefore, acephate has wide application and great demand. At present, the main process for preparing acephate is to first isomerize O, O-dimethylphosphoramide (spermine) to generate O, S-dimethylphosphoramide (methamidophos), and then acetyl into acephate. There will be many by-products in the whole process, the main by-product is O,O-dimethyl-N-acetylphosphorothioate, commonly know...

Claims

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Application Information

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IPC IPC(8): C07F9/24
Inventor 陈新志葛新
Owner ZHEJIANG UNIV
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