Method for closed-loop synthesis of nicosulfuron by using hydrogen sulfide

A technology of nicosulfuron and hydrogen sulfide, applied in the direction of organic chemistry, etc., can solve the problems of large amount of waste water, complex production process, poor controllability of process safety, etc., achieve high comprehensive utilization rate of resources, simple process equipment, improved The effect of the production environment
CN113461667AActive Publication Date: 2021-10-01ZIBO NAB AGROCHEM
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
ZIBO NAB AGROCHEM
Publication Date
2021-10-01

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Abstract

The invention belongs to the technical field of nicosulfuron original medicine production, and particularly relates to a method for closed-loop synthesis of nicosulfuron by using hydrogen sulfide, wherein the method comprises the following steps: reacting tetramethoxypropane with ethyl cyanoacetate to generate 1-cyano-4-methoxy-1-ethoxycarbonyl-1,3-butadiene (cyanoene for short, the same below); reacting cyano alkene with hydrogen sulfide to generate ethyl 2-mercaptonicotinate (sulfydryl substance for short) in a closed-loop manner; reacting the sulfydryl substance with dimethylamine, and then carrying out oxychlorination reaction to obtain sulfonyl chloride; carrying out ammonolysis reaction on the sulfonyl chloride and ammonia gas to obtain sulfonamide; and reacting sulfonamide with solid light and pyrilamine to obtain the nicosulfuron. According to the method for closed-loop synthesis of nicosulfuron by using hydrogen sulfide, each reaction step is mild and controllable, process equipment is simple, the production cost is low, the product quality is good, three wastes are reduced, energy is saved, the production environment is improved, and the goal of carbon neutralization is favorably realized.
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Description

technical field

[0001] The invention belongs to the technical field of producing nicosulfuron technical field, and in particular relates to a method for synthesizing nicosulfuron by hydrogen sulfide ring closure. Background technique

[0002] The trade name of Nicosulfuron is Yunongle. It is a high-efficiency selective post-emergence herbicide for corn fields. It is mainly used to control weeds in winter and spring corn fields. Its dosage is low, its effect is good, and it is safe for corn and the environment. The majority of farmers welcome that nicosulfuron is an important high-efficiency green herbicide, and its main synthesis routes are as follows:

[0003] (1) Urethane method route:

[0004] Using 2-chloronicotinic acid as the raw material, first react with thionyl chloride to generate 2-chloronicotinyl chloride, then react with dimethylamine to obtain the intermediate 2-chloronicotinamide; then react with sodium hydrosulfide to obtain mercapto The sulfhydryl compound...

Claims

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