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Chemical composite method for O, S-dimethyl-2, 2, 2-trichlorine-1-hydroxy ethyl amido phosphoric acid

A hydroxyethylamino phosphoric acid, chemical synthesis technology, applied to O, can solve the problems of limited use, high toxicity, etc., and achieve the effect of reducing the amount of use and reducing environmental pollution

Inactive Publication Date: 2010-03-17
WENZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because benzene is a volatile and highly toxic solvent, its use is limited

Method used

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  • Chemical composite method for O, S-dimethyl-2, 2, 2-trichlorine-1-hydroxy ethyl amido phosphoric acid
  • Chemical composite method for O, S-dimethyl-2, 2, 2-trichlorine-1-hydroxy ethyl amido phosphoric acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] Under stirring, add 1,2-dichloroethane (2ml), methylamine phosphine (0.05mmol) and Cu(OTf) 2 (0.01 mmol) was added dropwise chloroacetaldehyde (while controlling the temperature of the water bath at 45°C). After the addition is complete, continue heating, and after stirring for about 2 hours, the solvent is evaporated. After column separation, the yield was 47%.

Embodiment 2

[0011] Under stirring, add 1,2-dichloroethane (2ml), methylamine phosphine (0.05mmol) and Cu(OTf) 2 (0.005 mmol) was added dropwise chloroacetaldehyde (while controlling the temperature of the water bath at 48°C). After the addition is complete, continue heating, and after stirring for about 2.5 hours, the solvent is evaporated. After column separation, the yield was 39%.

Embodiment 3

[0013] Under stirring, add 1,2-dichloroethane (2ml), methylamine phosphine (0.05mmol) and Cu(OTf) 2 (0.015 mmol) was added dropwise chloroacetaldehyde (while controlling the temperature of the water bath below 40°C). After the addition is complete, continue heating, and after stirring for about 3 hours, the solvent is evaporated. After column separation, the yield was 46%.

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Abstract

The invention relates to a chemical composite method for O, S-dimethyl-2, 2, 2-trichlorine-1-hydroxy ethyl amido phosphoric acid, which is as follows: taking methylamine phosphine and chloral as mainraw materials, taking 1, 2-dichloroethane as organic solvent, reacting for 2-3 hours in the presence of a catalyzer Cu (OTf)2. As the chemical composite method uses 1, 2-dichloroethane with relativelysmaller toxicity for replacing benzene as organic solvent and the usage amount is greatly reduced; therefore, in the production process, the chemical composite method greatly reduces the pollution tothe environment and is worth to popularize.

Description

Technical field [0001] The invention relates to a chemical synthesis method of O,S-dimethyl-2,2,2-trichloro-1-hydroxyethylamino phosphoric acid. This method is suitable for synthesis of O,S-dimethyl-2,2,2-trichloro-1-hydroxyethylamino phosphoric acid with methylamine phosphine and chloroacetaldehyde as main raw materials. Background technique [0002] Phosphoramide pesticides are currently the most commonly used insecticides and acaricides, especially methylamine phosphine, which is currently the pesticide with the largest output and consumption. However, due to its high toxicity, it can cause poisoning to humans and animals, or excessive pesticide residues in agricultural products. In addition, methylamine phosphine is extremely soluble in water, and most of the pesticides are lost after application, causing soil and water pollution and destroying the ecological balance. Therefore, in the process of replacing highly toxic pesticides, there are constant calls for prohibition. ...

Claims

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Application Information

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IPC IPC(8): C07F9/24
Inventor 余小春钟平黄连根张小红陈小平杨芝萍汤日元李术艳任爱山
Owner WENZHOU UNIVERSITY
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