Method for synthesizing imidacloprid technical material
A synthetic method, imidacloprid technology, applied in botany equipment and methods, insecticides, animal repellents, etc., can solve problems such as unsatisfactory effects and complicated imidacloprid production methods, and achieve good quality of finished products, high efficiency, and production The effect of simple method
Inactive Publication Date: 2017-10-10
JIANGSU KESHENG CROP TECH +1
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[0003] The object of the present invention is to provide a kind of synthetic method of imidacloprid original medicine, aim at solving the problem that the preparation method of existing imidacloprid is complicated, and effect is not ideal
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[0014] In order to make the object, technical solution and advantages of the present invention more clear, the present invention will be further described in detail below in conjunction with the examples. It should be understood that the specific embodiments described here are only used to explain the present invention, not to limit the present invention.
[0015] The raw materials involved in the synthetic method of the original drug of imidacloprid provided by the embodiments of the present invention include:
[0016]
[0017] The synthetic method of the original drug of imidacloprid provided by the embodiments of the present invention comprises the following steps:
[0018] S101: Add 450ml of toluene and 24.0g of ENG into a 1000ml three-necked flask, stir evenly, heat the system to above 95°C, then add 6.6g of sodium hydroxide, heat up and reflux with water, remove all the toluene after adding water, and obtain ENG sodium Salt;
[0019] S102: Put the prepared ENG sodiu...
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The invention discloses a method for synthesizing an imidacloprid technical material. The method comprises the following steps: dissolving N-nitro-aminomidazolane and sodium hydroxide in water, and reacting to produce an aqueous solution of a N-nitro-aminomidazolane sodium salt; heating, performing reflux dehydration, and completely removing methylbenzene after dehydration is completed so as to obtain the N-nitro-aminomidazolane sodium salt; adding the N-nitro-aminomidazolane sodium salt into a container, stirring and raising the temperature, adding a butanone solution of 2-chloro-5-chloromethylpyridine and 1-methylimidazole or a base metal salt thereof, and reacting for 5-6 hours by maintaining the temperature; completely removing the butanone after the reaction is ended, and performing hot filtration at the temperature of 50-60 DEG C; adding the filter cake into a reactor, adding methylbenzene and butanone, heating, stirring and washing; cooling and filtering the system in a stirring state, thereby obtaining the imidacloprid technical material. According to the method disclosed by the invention, 'double pyrazole' impurities produced by a deep reaction carried out between imidacloprid and CCMP (Chloro-6-Trichloromethylpyridine) is controlled, so that alkaline hydrolysis of two reaction raw materials such as the CCMP and imidazolidine and the finished imidacloprid product is inhibited, the condensation yield is increased, and the method disclosed by the invention is simple in process, high in efficiency and high in finished product quality.
Description
technical field [0001] The invention belongs to the technical field of insecticides, and in particular relates to a synthesis method of imidacloprid active drug. Background technique [0002] In recent years, imidacloprid, as an ultra-efficient neonicotinoid insecticide, has the characteristics of broad-spectrum, high efficiency, low toxicity, and low residue. It is not easy for pests to develop resistance, and it is safe for humans, animals, plants, and natural enemies. And systemic absorption and other multiple effects. After the pests are exposed to the pesticide, the normal conduction of the central nervous system is blocked, causing them to paralyze and die. The product is quick-acting, and has a high control effect one day after application, and the residual period is as long as about 25 days. The efficacy and temperature are positively correlated, the higher the temperature, the better the insecticidal effect. It is mainly used to control piercing-sucking mouthpart...
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IPC IPC(8): C07D401/06A01N51/00A01P7/04
CPCC07D401/06A01N51/00
Inventor 吴重言吴伟吴静徐其文
Owner JIANGSU KESHENG CROP TECH