Process for synthesizing dimethoate

A synthetic method and technology of dimethoate, applied in the field of dimethoate synthesis, can solve the problems of unreported dimethoate synthesis method, insufficient yield and purity, low toxicity, etc., and achieve remarkable social benefits, high income, and small investment Effect

Inactive Publication Date: 2005-11-30
姚文刚
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its shortcoming is: the reaction condition is a two-phase system, and its yield and purity are not high enough
[0020] In 1993, U.S. Patent US5234919 "Preparation of Water-Soluble Highly Active Dimethoate" mixed dimethoate with various low-alkyl alcohols and acetate

Method used

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  • Process for synthesizing dimethoate
  • Process for synthesizing dimethoate
  • Process for synthesizing dimethoate

Examples

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preparation example Construction

[0027] (1) The preparation of the intermediate phosphorothioate of dimethoate

[0028] Reaction formula:

[0029]

[0030] M=NH 4 , Na, K, Li

[0031] Prepare 1 mol of phosphorothioate into a 38% organic solution, such as methanol, ethanol, isopropanol or tetrahydrofuran, and put it into a reaction tank with 1 to 4 mol of methyl chloroacetate, start stirring, heat up to 0 to 60°C, and React in phase, keep warm for 80-120 minutes, then filter and remove solvent to obtain phosphorothioate.

[0032] (2) Dimethoate is synthesized from phospholipid and methylamine as raw materials

[0033] Reaction formula:

[0034]

[0035] Brief description of the process:

[0036] Put 1 mol of phosphorothioate into the tank, under the condition of -10~5℃, add a solution containing 1.0~1.4mol of monomethylamine, such as methanol, ethanol, acetone, isopropanol or tetrahydrofuran, and a solution that can dissolve phosphoric acid Add the organic solvent of salt to the reaction system. Af...

Embodiment 1

[0038] Add 18.44 grams of 38% ammonium salt methanol solution into the reaction tank, start stirring, and when heated to 55±5°C, add 8.68 grams of methyl chloroacetate dropwise. ~2 hours. Generate 8.38 g of phosphorothioate.

[0039] Cool the prepared phosphorothioate to -10-0°C, add dropwise a methanol solution containing 1.13 g of monomethylamine under stirring to carry out aminolysis. During the aminolysis process, keep warm for 75 to 150 minutes. Remove solvent, obtain dimethoate pure product 8.17 grams. The total yield is 88.9%.

Embodiment 2

[0041] Add 20.57 grams of 35% sodium salt methanol solution into the reaction tank, start stirring, and when heated to 55±5°C, add 8.68 grams of methyl chloroacetate dropwise. ~2 hours. Generate 8.42 g of phosphorothioate.

[0042] The prepared phosphorothioate was cooled to -10-0°C, and a methanol solution containing 1.13 g of monomethylamine was added dropwise with stirring to carry out aminolysis. During the aminolysis process, keep warm for 75 to 150 minutes. Remove solvent, obtain dimethoate pure product 8.02 grams. The total yield is 89%.

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Abstract

The invention discloses a method for synthesizing dimethoate, which takes microcosmic salt and methyl chloroacetate as material to synthesize intermediate phosphate ester. The invention chooses phosphate ester and aminomethane as material to synthesize dimethoate. The reaction reacts in homogeneous system of organic solvent for 80-160 minutes in temperature of 0-60 DEG C. The invention synthesizes dimethoate in temperature of -10-5 DEG C for 60-150 minutes. Said microcosmic salt comprises ammonium salt, sodium salt, potassium salt and lithium salt. Said solvent comprises carbinol, alcohol, acetone, alcohol isopropylicum and tetrahydrofuran. The invention possesses carry out homogeneous phase reaction system to produce dimethoate with gross yield of up to 30% and pureness of 90% under the condition of existing device and material.

Description

technical field [0001] The invention relates to a method for synthesizing dimethoate, which belongs to the insecticide of organophosphorus compounds. Background technique [0002] Existing dimethoate synthetic method, once had a lot of technical data to report dimethoate at home and abroad in the fifties to the eighties described in the 139th page of new edition bound book " foreign pesticide kind manual " page 139 published by the Pesticide Information Center of the Ministry of Chemical Industry Synthetic methods, the main methods are: pre-amination method (chloroacetamide method), methyl isocyanate method, post-amination method. Adopt the front aminolysis method to prepare dimethoate, because side reaction is many, product yield and purity are all lower, and adopt methyl isocyanate method to prepare dimethoate, because it is solid-liquid heterogeneous system reaction, process condition is not easy Control has a greater impact on product purity. Moreover, the raw material...

Claims

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Application Information

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IPC IPC(8): C07F9/22
Inventor 姚文刚
Owner 姚文刚
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