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Preparation method of deuterated methyl parathion

A technology of deuterated methyl parathion and deuterated methanol, applied in the field of chemical analysis, can solve problems such as lack of complete and detailed literature reports, and achieve the effects of good product quality, mild reaction conditions and simple operation

Active Publication Date: 2018-11-09
公安部鉴定中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] About the synthesis of deuterated methyl parathion (formula compound V), there is no complete and detailed literature report at present

Method used

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  • Preparation method of deuterated methyl parathion
  • Preparation method of deuterated methyl parathion
  • Preparation method of deuterated methyl parathion

Examples

Experimental program
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Embodiment 1

[0040] (1) Phosphor trichloride monoesterifies with deuterated methanol to obtain reaction product II (molecular weight 169.979)

[0041]

[0042] Weigh 20.8g of phosphorus trichloride (compound I, 122.4mmol) into a 100mL round-bottomed flask, cool to -10°C in an ice-salt bath, then add 13.3g of deuterated methanol (367.2mmol) dropwise, in 15-20min After the dropwise addition, raise the temperature to -5°C and continue stirring for 1 hour, add 50 mL of ice water (water at 0°C) to the reaction system, stir for 5 minutes, then separate the liquids, keep the organic phase after liquid separation, and use the water phase after liquid separation Dichloromethane was extracted twice, each with 20 mL of dichloromethane. Combine the organic phase after liquid separation and the organic phase obtained by extraction, dry with 25g of anhydrous magnesium sulfate, filter and concentrate under reduced pressure to obtain reactant II, which is O-(methyl-D3)-thiophosphoryl di chlorine.

[...

Embodiment 2

[0051] (1) Phosphor trichloride monoesterifies with deuterated methanol to obtain reaction product II

[0052]

[0053] Weigh 20.8g of phosphorus trichloride (compound I, 122.4mmol) into a 100mL round-bottomed flask, cool to -10°C in an ice-salt bath, then add 13.3g of deuterated methanol (367.2mmol) dropwise, in 15-20min After the dropwise addition, raise the temperature to -5°C and continue stirring for 1 hour, add 50 mL of ice water (water at 0°C) to the reaction system, stir for 5 minutes, then separate the liquids, keep the organic phase after liquid separation, and use the water phase after liquid separation Extract twice with dichloromethane, each extraction with 20 mL of dichloromethane. Combine the organic phase after liquid separation and the organic phase obtained by extraction, dry with 25g of anhydrous magnesium sulfate, filter and concentrate under reduced pressure to obtain reactant II, which is O-(methyl-D3)-thiophosphoryl di chlorine.

[0054] (2) The rea...

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Abstract

The invention discloses a preparation method of deuterated methyl parathion. The preparation method comprises the following steps: (1) performing the mono-esterification for thiophosphoryl chloride and deuterated methanol, and obtaining a reaction product II; (2) performing the esterification for the reaction product II and p-nitrophenol, and obtaining a reaction product IV; and (3) performing theesterification for the reaction product IV and deuterated methanol, obtaining a reaction product V, wherein the reaction product V is the deuterated methyl parathion. The invention provides a novel method for synthesizing the deuterated methyl parathion. The method has the advantages of moderate reaction condition, simple operation, good quality of deuterated methyl parathion product, good stability and the like.

Description

technical field [0001] The invention relates to the technical field of chemical analysis. Specifically, it is a preparation method of deuterated methyl parathion. Background technique [0002] Methyl parathion commonly known as methyl 1605 (formula compound Va), scientific name O, O-dimethyl-O-(4-nitrophenyl) phosphorothioate, an organophosphorus insecticide, is highly toxic grade pesticides. my country is a large agricultural country, and the use of pesticides is large. Organophosphorus insecticides have a wide range of applications and high toxicity. In recent years, criminal cases such as poisoning, suicide, and misuse caused by such drugs have occurred from time to time. This requires the public security judicial appraisal department to test the samples of samples involving such drugs. In order to ensure the preparation and reliability of the detection method, the internal standard is added during the detection, and the corresponding deuterium is the best internal st...

Claims

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Application Information

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IPC IPC(8): C07F9/18C07B59/00
CPCC07B59/004C07F9/18C07B2200/05
Inventor 杜鸿雁徐小英魏春明宋歌于忠山董颖王瑞花董林沛
Owner 公安部鉴定中心
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