Synthesis method of glufosinate-ammonium intermediate methylphosphorus dichloride

A technology for the synthesis of methyl phosphorus dichloride and the synthesis method, which is applied in the field of synthesis of glufosinate-ammonium intermediate methyl phosphorus dichloride, can solve the problems of increasing solvent and raw material recovery costs, consuming large solvents, etc., and achieve reduction of recovery Difficulty, the effect of improving product purity and avoiding the use of solvents

Inactive Publication Date: 2016-10-26
ANHUI COSTAR BIOCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method needs to consume a large amount of solvent, and the unreacted phosphorus trichlo

Method used

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  • Synthesis method of glufosinate-ammonium intermediate methylphosphorus dichloride

Examples

Experimental program
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Effect test

Embodiment 1

[0012] Example 1: Add aluminum trichloride and phosphorus trichloride in a closed reactor according to the molar ratio of 1:3, vacuumize to remove the air, stir evenly and then feed in methyl chloride, the molar amount of methyl chloride is aluminum trichloride 2 times, the material is heated to 85 ° C, and then inert nitrogen is passed through to pressurize to 1.5 MPa. The reaction was stopped after 8 hours, the temperature was raised to 100-120°C to remove excess phosphorus trichloride, and the solid was fully dried.

[0013] After heating the ternary complex to a temperature of 140-150° C., adding aluminum powder and sodium chloride, distilling while reacting to obtain methyl phosphorus dichloride, the purity is 99.0%, and the yield is 85.0%.

Embodiment 2

[0014] Example 2: Add aluminum trichloride and phosphorus trichloride in a closed reactor according to the molar ratio of 1:2, vacuumize to remove the air, stir evenly and then feed in methyl chloride, the molar amount of methyl chloride is aluminum trichloride 2 times, the material is heated to 85 ° C, and then inert nitrogen is passed through to pressurize to 1.5 MPa. The reaction was stopped after 8 hours, the temperature was raised to 100-120°C to remove excess phosphorus trichloride, and the solid was fully dried.

[0015] After the ternary complex is heated to a temperature of 140-150°C, aluminum powder and sodium chloride are added, and distilled while reacting to obtain methyl phosphorus dichloride with a purity of 98.5% and a yield of 69.6%.

Embodiment 3

[0016] Example 3: Add aluminum trichloride and phosphorus trichloride in a closed reactor according to the molar ratio of 1:5, vacuumize to remove the air, stir evenly and then feed in methyl chloride, the molar amount of methyl chloride is aluminum trichloride 2 times, the material is heated to 85 ° C, and then inert nitrogen is passed through to pressurize to 1.5 MPa. The reaction was stopped after 8 hours, the temperature was raised to 100-120°C to remove excess phosphorus trichloride, and the solid was fully dried.

[0017] After the ternary complex is heated to a temperature of 140-150°C, aluminum powder and sodium chloride are added, and distilled while reacting to obtain methyl phosphorus dichloride with a purity of 99.4% and a yield of 83.7%.

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Abstract

The invention discloses a synthesis method of glufosinate-ammonium intermediate methylphosphorus dichloride, belonging to the technical field of synthesis of a glufosinate-ammonium intermediate. The synthesis method comprises the following steps: by using methyl chloride, aluminum trichloride and phosphorus trichloride as raw materials, carrying out reaction under the pressure of 0.5-3.0 MPa for 6.5-10 hours to obtain a ternary complex, adding aluminum powder and sodium chloride, and carrying out reaction at a certain temperature to obtain the methylphosphorus dichloride. According to the method, the phosphorus trichloride is simultaneously used as the reactant and solvent; and the reaction pressure is enhanced, so that the methyl chloride gas sufficiently reacts with the solid and liquid phases without adding any other solvent, thereby enhancing the product purity, avoiding the problems of solvent separation, recovery and the like, reducing the phosphorus trichloride recovery difficulty, and greatly lowering the production cost.

Description

Technical field: [0001] The invention belongs to the technical field of synthesis of glufosinate-ammonium intermediates, in particular to a method for synthesizing methyl phosphorus dichloride of glufosinate-ammonium intermediates. Background technique: [0002] Methyl phosphorus dichloride is a colorless, transparent liquid with a strong pungent odor. It is very easy to absorb water, and it reacts with water to exotherm violently and even burns. It is an important chemical intermediate and can be used in organic synthesis, pharmaceuticals, pesticides, In addition, methyl phosphorus dichloride is also an important intermediate for the preparation of new high-efficiency pesticide glufosinate-ammonium. [0003] The synthesis methods of methyl phosphorus dichloride reported so far include methane method, methyl iodide complexation method, methyl chloride complexation method and some other synthetic methods. Patent US4101573 discloses a carbon tetrachloride as an initiator, met...

Claims

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Application Information

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IPC IPC(8): C07F9/52
CPCC07F9/52C07F9/509
Inventor 史玉龙王佳袁晓路胡其钊钱前黄成强
Owner ANHUI COSTAR BIOCHEM CO LTD
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