Method for preparing neonicotine pesticide clothianidin

A technology of neonicotinoids and clothianidin, which is applied in the fields of insecticides and organic chemistry, can solve the problems of special reaction conditions, low purity of clothianidin, and difficulty in industrialization, and achieve short reaction time, high selectivity, The effect of mild reaction conditions

Inactive Publication Date: 2012-05-02
SHANDONG JINGPENG BIO PESTICIDE
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Problems solved by technology

[0004] At present, the existing clothianidin preparation method: 1.5-aminomethyl-2-chlorothiazole reacts with 1.2-dimethyl-3-nitroisothiourea to generate clothianidin; 2.2-chloro-5-chloromethylthiazole React with N-methyl-N-nitroguanidine to generate clothianidin; 3. 2-chloro-5-chloromethylthiazole reacts with 2-methyl-N-nitroisothiourea to obtain 1-(2-chloro -thiazole methyl)-3-nitro-2-methylisothiourea reacts with methylamine solution to generate clothianidin, and the above-mentioned methods for preparing clothianidin all have low selectivity, special reaction conditions, long reaction time, The prepared clothianidin has low purity and is not easy to realize the defects of industrialization

Method used

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  • Method for preparing neonicotine pesticide clothianidin
  • Method for preparing neonicotine pesticide clothianidin
  • Method for preparing neonicotine pesticide clothianidin

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Embodiment 1

[0028] The preparation method of the neonicotinoid insecticide clothianidin of the present embodiment comprises the following technical process:

[0029] 1. Synthesis of intermediate 1.5-dimethyl-2-nitroimino-hexahydro-1.3.5-triazine

[0030] (1), ring formation reaction

[0031] Put methanol into the reaction kettle, start stirring, add methylguanidine, close the hand hole, pump in monomethylamine and formaldehyde, the weight ratio of methanol, methylguanidine, monomethylamine and formaldehyde is (0.8-1.2): (1.5-1.9): (3.2-3.6): (0.4-0.6), slowly raise the temperature to 40-60°C, stir and react for 3-7 hours, take samples for testing, the standard for the completion of the reaction is that the reaction solution contains 2% formazan base guanidine;

[0032] (2), concentration, crystallization, filtration

[0033] The temperature of the reaction liquid in the reaction kettle is lowered to 20-40°C, the vacuum degree in the kettle is controlled at 0.08-0.10Mpa, and the meth...

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Abstract

The invention relates to a method for preparing a neonicotine pesticide clothianidin and belongs to the technical field of a pesticide. The method comprises the following steps of: 1, synthetizing an intermediate 1,5-dimethyl-2-nitryl imido-hexahydro-1,3,5-triazine; 2, synthetizing an intermediate 1-(2-chloro thiazole-5-methyl-2-nitryl imido-3,5-dimethyl-hexahydro-1,3,5-triazine (which is called as TST for short); and 3, synthetizing the clothianidin. In the method for preparing the neonicotine pesticide clothianidin, which is disclosed by the invention, the clothianidin is generated by decomposing 1-(2-chloro thiazole-5-methyl-2-nitryl imido-3,5-dimethyl-hexahydro-1,3,5-triazine, and the clothianidin with purity content of higher than or equal to 95 percent can be prepared. The method has the advantages of high selectivity, mild reaction condition, short reaction time, high product purity and easiness in realizing industrialization.

Description

technical field [0001] The invention relates to a preparation method of a neonicotinoid insecticide clothianidin, which belongs to the technical field of pesticides and insecticides. Background technique [0002] Neonicotinoid insecticides are inhibitors of insect nicotinic acetylcholine receptors, and are the fourth generation of novel insecticides following organophosphorus, carbamate, and pyrethroid insecticides. It is an invention of great significance in the research field. This type of insecticide has high activity, wide insecticidal spectrum, is safe for mammals and aquatic animals, and has good system properties and environmental friendliness. There is no cross-resistance between traditional pesticides. Therefore, it is currently the most important class to replace highly toxic insecticides. [0003] Clothianidin is a neonicotinoid insecticide developed and applied by Bayer in 1996. Its mechanism of action is similar to other neonicotinoid insecticides. It is mainly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/32A01P7/04
Inventor 张毅
Owner SHANDONG JINGPENG BIO PESTICIDE
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