Method for preparing pesticide nitenpyram

A technology of nitenpyram and insecticide, which is applied in the field of preparation of nitenpyram, can solve the problems of low yield, unsafe operation, complicated preparation process, etc., and achieve industrial production, reduce environmental pollution, and produce The effect of high purity

Active Publication Date: 2012-12-12
浙江禾本科技股份有限公司
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  • Abstract
  • Description
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Problems solved by technology

Many problems were encountered in the test: the preparation process of the intermediate 1,1-dimethylthio-2-nitroethylene is complex, and it is toxic and has an unpleasant odor. There are complex process flow, unsafe operation, pollution of the environment, Disadvantages such as high cost; ② using documented technology to prepare 1,1,1-trichloro-2-nitroethane with industrial hydrochloric acid and nitric acid, and then react with N

Method used

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  • Method for preparing pesticide nitenpyram
  • Method for preparing pesticide nitenpyram
  • Method for preparing pesticide nitenpyram

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Embodiment Construction

[0030] The present invention will be described in further detail below in conjunction with the accompanying drawings and embodiments.

[0031] Such as figure 1 Shown, present embodiment is carried out by following synthesis process route and step:

[0032] (1) elimination reaction, its reaction equation is:,

[0033]

[0034] The elimination reaction is carried out according to the following steps: in a 2000L enamel reaction kettle, add 450Kg1,1,2-trichloroethane, heat to a certain temperature, and evenly add 30% sodium hydroxide solution dropwise under vigorous stirring 450Kg, the dropping time is about 5 hours. During the reaction, the product vinylidene chloride escapes from the top of the distillation column, the temperature of the column top is 32-40°C, and enters the receiving tank after being condensed by the condenser tube. After dropping, continue the insulation reaction until substantially no product escapes. Then slowly raise the temperature to a certain temp...

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Abstract

The invention relates to a method for synthesizing a pesticide, and in particular relates to a method for preparing a pesticide nitenpyram. The method for preparing the pesticide nitenpyram is characterized in that 1, 1, 1, 2-trichloroethane is taken as a starting material, and an intermediate of 1, 1, 1-trichloro-2-nitroethane is directly synthesized through elimination reaction and catalytical nitration reaction; 2, 2-chloro-5-nitrapyrin is taken as a staring material, water is taken as solvent, a phase-transfer catalysis technology is adopted, and an intermediate of N-ethyl-2-chloro-5-pyridyl methyl amine is obtained through N-alkylation reaction; and 3, the two intermediates are mixed together, dichloromethane with low toxicity is taken as the solvent, condensation and methyl amination reaction are carried out in a same reaction vessel, and the nitenpyram is produced through extracting, desolventizing and crystallizing. The method for preparing the pesticide nitenpyram has high product yield and purity and a short technological process. Compared with the prior art, the method has the advantages of high total yield, low cost, high product purity, less environmental pollution, benefits for industrial production and the like.

Description

technical field [0001] The invention relates to a method for synthesizing insecticides, in particular to a method for preparing nitenpyram with 1,1,2-trichloroethane and 2-chloromethylpyridine as main raw materials. Background technique [0002] Nitenpyram is a new generation of neonicotinoid insecticides following imidacloprid, and its molecular structure is: [0003] [0004] It is the latest domestically popularized new variety to replace highly toxic organophosphorus pesticides. It has unique chemical and biological properties and has a nerve-blocking effect on synaptic receptors of pests. It is effective against various aphids, whiteflies, rice leafhoppers and thistles. Horses and others have shown excellent activity, and have the advantages of high efficiency, low toxicity, environmental safety, high systemicity, no cross-resistance, and no phytotoxicity to crops. crop pests. In particular, this product has a lore killing effect on SBPH and BPH. It takes about 10 ...

Claims

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Application Information

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IPC IPC(8): C07D213/61
Inventor 曾挺陈华陈共华潘光飞
Owner 浙江禾本科技股份有限公司
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