111991-09-4Relevant articles and documents
Method for closed-loop synthesis of nicosulfuron by using hydrogen sulfide
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, (2021/10/05)
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.
Nicosulfuron water-phase method synthesis process
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Paragraph 0020-0031, (2021/04/14)
The present invention relates to the technical field of pesticides, and provides a nicosulfuron water-phase method synthesis process, which comprises: S1, material feeding: adding 2-ethoxycarbonyl amino sulfonyl-N, N-dimethyl nicotinamide, 2-amino-4, 6-dimethoxypyrimidine, a phase transfer catalyst and a solvent to a reaction kettle, and starting stirring; S2, reacting at the temperature of 60-100 DEG C for 5-7 hours; and S3, discharging: centrifuging and drying to obtain the nicosulfuron. Through the technical scheme, the problems of complex process and poor product quality in the prior art are solved.
Preparation method of nicosulfuron crude drug
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Paragraph 0020; 0024; 0026; 0030; 0031; 0035, (2020/03/23)
The preparation method, of the nicosulfuron crude drug comprises the following steps: synthesizing, isocyanate group sulfonyl - NNNN, N-dimethyl nicotinamide: triphosgene 2 - triethylamine and 2 - amino - 4444, 6-dimethoxypyrimidine as main raw materials in, reaction to synthesize nicosulfuron-N, N-dimethylnicotinamide 0-80 °C and 2 - amino - 4444, 6-dimethoxypyrimidine as main raw materials to synthesize nicosulfuron-N, N-dimethylaminopyridine as a main, raw material, and high yield; of nicosulfuron. 2 - The method provided by the invention comprises the following steps, synthesizing 2 - 2 -isocyanuric acid group, sulfonyl - NNNNor N-dimethylaminopyrimidinil in 0-100 °C reaction to form a nicosulfuron prodrug. by reacting. 2 - The preparation method comprises the following. steps, synthesizing nicosulfuron-N, N-dimethyl nicotinamide.
Preparation method of nicosulfuron
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Paragraph 0030-0033, (2020/07/02)
The invention discloses a preparation method of nicosulfuron. The method comprises the following steps: carrying out first reaction treatment on 2-sulfamoyl-N,N-dimethylformamide to obtain corresponding carbamate, and carrying out a second reaction on the carbamate and dimethoxyaminopyrimidine to obtain the nicosulfuron. On the basis of the prior art, by improving the technological process, the yield of the intermediate 2-sulfamoyl-N,N-dimethylnicotinamide is increased, that is, the yield of nicosulfuron can be effectively increased; and meanwhile, the adopted raw material 2-chloro-N,N-dimethylnicotinamide can effectively reduce the cost so as to meet the requirements of modern industrial production.
Nicosulfuron crystalline hydrate as well as preparation method and application thereof
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Paragraph 0050; 0051; 0064-0069, (2019/10/23)
The invention provides nicosulfuron crystalline hydrate as well as a preparation method and the application thereof and belongs to the field of organic synthesis. The invention provides the nicosulfuron crystalline hydrate which has a good crystal form, does not absorb moisture or damp in the air, is good in stability and easy in drying and later processing, in addition, the product is high in chemical purity, uniform in granularity distribution and good in dispersibility, a preparation processed later is good in stability, rapid in disintegration speed, high in bioactivity, remarkable in quality advantage, free of phenomena of material moisture absorption and sticking in the process of drying, crushing, packaging and downstream preparation processing in production workshops, beneficial toclean production and preparation material blending uniformity, and in addition has the advantages of being simple and easy in production process, high in yield, low in cost, and the like.
Synthesizing method of raw nicosulfuron
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Paragraph 0013; 0024; 0035-0038; 0043-0044; 0049-0050; 0055, (2018/10/19)
The invention provides a synthesizing method of raw nicosulfuron. The method includes: synthesizing N,N-dimethyl nicotinamide, oxidizing the N,N-dimethyl nicotinamide, performing the sulfonylation of2-carbamido-4,6-dimethoxy pyrimidine, and synthesizing the raw nicosulfuron. The synthesizing method is short in synthesizing route, low in cost, high in yield, mild in synthesizing conditions, capable of avoiding the use of high-toxicity and high-pollution raw materials such as phosphorus oxychloride, chlorine and phosgene, green and safe, and capable of achieving industrial production.
Synthesizing technology and device for improving nicosulfuron purity
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Paragraph 0013; 0014; 0015, (2018/03/24)
The invention relates to a synthesizing technology and device for improving nicosulfuron purity. The technology is characterized in that 3-[(N,N-dimethylaminocarbonyl)-2-pyridyl] sulfonylcarbamate, 4,6-dimethoxy-2-pyrilamine and methylbenzene are heated to condense; mixed steam of methylbenzene treated as a solvent in the reaction and ethyl alcohol produced in the condensation enters a condenser;the mixed solution of condensed methylbenzene and ethyl alcohol enters an absorbent storing tank; methylbenzene absorbed through the ethyl alcohol is heated through an absorbent, and then the methylbenzene is added to a reaction kettle; the reaction is stopped when the content of the ethyl alcohol in the mixed steam produced by the reaction kettle is less than 0.0005%; the mixed solution in the reaction is cooled and centrifuged to obtain nicosulfuron. According to the technology, the ethyl alcohol produced in the reaction can be quickly and effectively removed, and the reaction is promoted to forwards perform, thus the purity and the yield of nicosulfuron can be improved; and moreover, the methylbenzene treated as the solvent and taken out through the ethyl alcohol is recycled, so that more energy is saved; and the reaction cycle is greatly reduced through the design, and as a result, the production efficiency is improved.
Synthesis process of nicosulfuron original medicine
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, (2017/08/29)
The invention relates to a synthesis process of a nicosulfuron original medicine. In the method, 2-chloronicotinic acid is used as a raw material to synthesize an intermediate 2-sulfunylchloro-N,N-dimethyl nicotinamide, which is then reacted with amino pyrimidine to produce the nicosulfuron. The method has good atom economy and meanwhile avoids use of highly-toxic raw materials, such as phosgene, and expensive catalysts. The method has simple operations, is low in pollution and is low in cost; by means of continuous material feeding and continuous distillation, continuous synthesis of the nicosulfuron original medicine is achieved, and synthesis quality and yield of the nicosulfuron are greatly improved.
Nicosulfuron method for the preparation of
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Paragraph 0023-0027, (2017/02/23)
The invention discloses a nicosulfuron preparation method. According to the invention, in an organic solvent, 2-sulfonyl chloride-N,N-dimethyl nicotinamide and sodium cyanate are subjected to a reaction for 2-10h under stirring under the existence of organic alkali and under a temperature of 10-50 DEG C; 2-amino-4-dimethoxy pyrimidin is added, and a reaction is carried out for 0.5-5h under stirring under an environmental temperature, such that nicosulfuron is obtained. According to the invention, sodium cyanate is subjected to a reaction with 2-sulfonyl chloride-N,N-dimethyl nicotinamide to produce corresponding isocyanate, and isocyanate is subjected to a condensation reaction with 2-amino-4-dimethoxy pyrimidin. The synthetic route has the advantages of mild reaction condition, low cost, high yield, and high purity. The intermediate is not needed to be separated, and reaction period is short, such that the method is suitable for industrialized productions. The method also has the advantages of low toxicity and no environment pollution, such that the method satisfies a green chemistry principle.
METHOD FOR PRODUCING PYRIMIDINE COMPOUND
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Page/Page column 16, (2011/01/11)
To provide a method for producing pyrimidine compound useful as an intermediate for agricultural chemicals or pharmaceuticals, which is simple in operation, presents high yield and produces only a small amount of by-products. The method comprises reacting a compound represented by the formula (I) with a compound represented by the formula (II) in the presence of a pyridine compound to produce a compound represented by the formula (III), a compound represented by the formula (IV) or their mixture.
