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Preparation method of nitenpyram

A technology of nitenpyram and monomethylamine, which is applied in the field of preparation of nitenpyram, can solve the problems of high environmental protection pressure, difficult recovery, low reaction yield, etc., and achieves mild reaction conditions, green process, and high reaction yield. high rate effect

Inactive Publication Date: 2018-11-16
SHANGHAI JINJING CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] This route uses hydrochloric acid and nitric acid for nitration, a large amount of acid is used, the waste acid is difficult to handle, the environmental protection pressure is high, the amount of solvent in the condensation process is large, the recovery is difficult, causing environmental pollution, and the product purification requires column chromatography, and the reaction yield is low. , high cost, not suitable for industrial production

Method used

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  • Preparation method of nitenpyram
  • Preparation method of nitenpyram
  • Preparation method of nitenpyram

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Embodiment 1

[0029] The preparation of embodiment 1 nitenpyram compound (I)

[0030] Put 1200kg of dichloromethane into a 2000L reactor, add 171kg (1kmol) of N-ethyl-2-chloro-5-pyridinemethanamine under stirring, 60L ion exchange resin 201x7, cool to internal temperature -10°C, drop 1 , A solution of 157kg (1.1kmol) of 1-dichloro-2-nitroethylene and 320kg of dichloromethane was added dropwise in 3 hours, and the internal temperature was controlled below 0°C. After dropping, keep warm at 0°C for 3 hours. After the reaction is complete, a solution containing compound (II) is obtained. Continue to lower the temperature of this solution to the internal temperature of -10°C, slowly pass in 46.5kg (1.5kmol) of monomethylamine gas, control the internal temperature below 0°C, and feed the calculated amount of monomethylamine gas for 3 hours, then keep warm at 0°C for reaction 3 hours. Complete, filter, wash the ion exchange resin with dichloromethane, concentrate the filtrate to dryness, add 28...

Embodiment 2

[0031] The preparation of embodiment 2 nitenpyram compound (I)

[0032] Put 1200kg of chloroform into the 2000L reaction kettle, throw in 171kg (1kmol) of N-ethyl-2-chloro-5-pyridinemethanamine under stirring, 70L ion exchange resin D201, cool to the inner temperature of 0°C, and drop 1,1- The solution of 142kg (1kmol) of dichloro-2-nitroethylene and 320kg of chloroform was added dropwise in 3 hours, and the internal temperature was controlled below 10°C. After dropping, the temperature was raised and kept at 20° C. for 3 hours. After the reaction is complete, a solution containing compound (II) is obtained. Continue to lower the temperature of the solution to an internal temperature of 0°C, slowly pass in 31kg (1kmol) of monomethylamine gas, control the internal temperature below 10°C, and feed the calculated amount of monomethylamine gas for 3 hours, then keep the temperature at 20°C for 3 hours. Complete, filter, dichloromethane washes the ion exchange resin, concentrates...

Embodiment 3

[0033] The preparation of embodiment 3 nitenpyram compound (I)

[0034] Put 1200kg of dichloroethane into the 2000L reactor, add 171kg (1koml) of N-ethyl-2-chloro-5-pyridinemethanamine under stirring, 60L ion exchange resin D301, cool to the inner temperature of 20°C, drop 1 , A solution of 170kg (1.2koml) of 1-dichloro-2-nitroethylene and 320kg of dichloroethane was added dropwise in 3 hours, and the internal temperature was controlled below 25°C. After dropping, the temperature was raised to 40°C and the reaction was kept for 2 hours. After the reaction is complete, a solution containing compound (II) is obtained. Continue to lower the temperature of this solution to an internal temperature of 20°C, slowly drop in 155kg (2kmol) of 40% monomethylamine solution, control the internal temperature below 25°C, finish the dripping in 3 hours, then raise the temperature to 40°C and keep it warm for 2 hours. Complete, filter, wash the ion exchange resin with dichloromethane, separa...

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Abstract

The invention discloses a preparation method of nitenpyram. The method comprises the steps: carrying out a catalytic reaction in a low-grade chlorinated hydrocarbon solvent by taking N-ethyl-2-chloro-5-pyridinemethylamine and 1,1-dichloro-2-nitroethylene as starting raw materials and anion exchange resin as an acid binding catalyst, ending the reaction, and carrying out filtration to remove the anion exchange resin to obtain a solution of an intermediate compound (II); introducing methylamine gases to the solution of the intermediate compound (II), ending the reaction, and carrying out filtration; and concentrating a filtrate, and separating out a crystal to obtain a target compound (I). The invention provides the preparation method of a synthesis process of nitenpyram, the preparation method is few in reaction steps, simple in process as well as green and environment-friendly in process, and nitenpyram is high in yield and quality. Compared with an existing technical process, the preparation method is simple and convenient in process operation, low in operation cost, free of wastewater discharge, capable of realizing recycle of the catalyst, green and environment-friendly in process, high in product quality and yield, low in cost, very suitable for industrial production and extremely high in industrial application value.

Description

technical field [0001] The invention belongs to the technical field of pesticide synthesis, and in particular relates to a preparation method of nitenpyram. Background technique [0002] Nitenpyram is a new generation of neonicotinoid insecticides following imidacloprid. It has the characteristics of high efficiency, low toxicity, systemic absorption, and no cross-resistance. It is an excellent control agent for homopteran pests. Nitenpyram is a new The mechanism of action of nicotinic insecticides is that it mainly acts on insect nerves, inhibits the activity of acetylcholinesterase, acts on cholinergic receptors, directly stimulates the neuromuscular junction of parasympathetic vegetative ganglia, and affects the nerve axons of insects. Touch receptors have a nerve blocking effect. It has good systemic and osmotic effects, low toxicity, high efficiency, broad spectrum, long-lasting effect, and no harm to crops. This product was successfully developed in 1989 by Takeda Co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/61
CPCC07D213/61Y02P20/584
Inventor 陈学军马俊唐松青
Owner SHANGHAI JINJING CHEM CO LTD
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