Preparation method of buprofezin

A technology of buprofezin and solvents, which is applied in the field of preparation of pesticide raw materials, can solve the problems of difficulty in raw material procurement and treatment of three wastes, and achieve the effects of reduced risk, low cost and high quality

Active Publication Date: 2011-02-16
LIANYUNGANG JINDUN AGROCHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Now the country prohibits the use of carbon tetrachloride, and toluene is a precursor chemical, and a variety of solvents are used in the production process, which i

Method used

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  • Preparation method of buprofezin
  • Preparation method of buprofezin
  • Preparation method of buprofezin

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0024] Example 1. A method for preparing buprofezin, in which chlorobenzene is uniformly used as a solvent in all reaction steps requiring a solvent in the process of preparing buprofezin.

Embodiment 2

[0025] Example 2. A kind of preparation method of Buprofezin described in embodiment 1, concrete steps are as follows:

[0026] (1) Preparation of tert-butyl isothiocyanate: Add ammonium thiocyanate to water, the weight ratio of ammonium thiocyanate to water is 1:0.5, stir to dissolve; then add tert-butanol, stir for 10 minutes , the molar ratio of tert-butanol to ammonium thiocyanate is 1:0.9; the temperature is slowly raised to 70°C, and then industrial hydrochloric acid is added dropwise under reflux for 1 hour, and the molar ratio of tert-butanol to hydrochloric acid is 1: 1. After the dropwise addition, keep warm for 2 hours under reflux; then lower the temperature to 40°C, separate layers, and the acidic wastewater goes to the wastewater treatment tank, and the upper oil layer is washed with alkaline aqueous solution. The molar ratio is 1:0.1, and then washed with water to pH6.8, the light yellow oil layer liquid is returned to the reaction kettle equipped with the refl...

Embodiment 3

[0030] Example 3. A kind of preparation method of Buprofezin described in embodiment 1, concrete steps are as follows:

[0031](1) Preparation of tert-butyl isothiocyanate: Add ammonium thiocyanate to water, the weight ratio of ammonium thiocyanate to water is 1:2, stir to dissolve; then add tert-butanol and stir for 40 minutes , the mol ratio of tert-butanol to ammonium thiocyanate is 1: 1.2; slowly warming up to 90°C, then dropwise add industrial hydrochloric acid under reflux, the time of addition is 3 hours, the mol ratio of tert-butanol to hydrochloric acid is 1: 2.0, keep warm for 4 hours under reflux after the dropwise addition; then cool down to 70°C, stratify, acid waste water goes to the waste water treatment tank, and the upper oil layer is washed with alkaline aqueous solution, the alkaline substances in the alkaline aqueous solution are mixed with tert-butanol The molar ratio is 1: 0.5, and then washed to pH7.2, the light yellow oil layer liquid is returned to th...

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Abstract

The invention discloses a preparation method of buprofezin, which is characterized in that chlorobenzene is uniformly used as a solvent in all reaction steps requiring the solvent. The preparation method specifically comprises the steps of preparation of isosulfocyanic acid butyl ester, preparation of a 1-isopropyl-3-tert-butyl thiourea solution, preparation of an N-chloromethyl-N-phenyl carbamyl chloride solution and preparation of raw buprofezin powder. In the invention, the chlorobenzene is uniformly used as the solvent in all steps requiring the solvent for preparing the buprofezin so that dangers are reduced in a production process in a production department, the purpose of environmental-friendliness is achieved, and product quality reaches an international standard. The preparation method in the invention is simple, convenient, environmental-friendly and more reasonable, has low cost and high quality, and is more suitable for industrialized production. The total reaction yield of the method can reach more than 68.5% if taking ammonium thiocyanate as reference.

Description

technical field [0001] The invention relates to a method for preparing pesticide raw materials, in particular to a method for preparing buprofezin. Background technique [0002] Buprofezin, whose chemical name is 2-tertbutylimino-3-isopropyl-5-phenyl-1,3,5-thiadiazin-4-one, is a thiadiazine insect growth regulator agent, an insect molting inhibitor. By inhibiting the synthesis of chitin and interfering with metabolism, the pests cannot molt and metamorphosis normally and gradually die. It has the characteristics of high activity, high selectivity and long residual period. It is a chitin synthesis inhibitor of heterocyclic insects with strong contact and stomach toxicity and permeability; it does not kill adults, but can reduce oviposition and hinder egg hatching. [0003] Buprofezin is an agricultural insecticide with persistent larvicidal activity against Coleoptera, some Homoptera and Acarina. It can effectively control Leafhoppers and Planthoppers on rice; Leafhoppers...

Claims

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Application Information

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IPC IPC(8): C07D285/34
Inventor 王耀良石卫兵
Owner LIANYUNGANG JINDUN AGROCHEMICAL CO LTD
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