1694-92-4Relevant articles and documents
Industrial production method of o-nitrobenzenesulfonyl chloride
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Paragraph 0052; 0056-0058; 0059; 0063-0065, (2019/10/01)
The invention discloses an industrial production method of o-nitrobenzenesulfonyl chloride. The method comprises the following steps that o-nitrochlorobenzene and sodium methyl mercaptide are subjected to an etherification reaction, filtering is conducted, an obtained filter cake is subjected to recrystallization, and through centrifugation separation and drying, a dry product of o-nitrobenzene dimethyl sulfide is obtained; the dry product of o-nitrobenzene dimethyl sulfide is subjected to a chlorination reaction in batches to obtain a wet crude product, an appropriate amount of hydrochloric acid is added in a chlorination reaction system, the chlorination reaction is carried out in a hydrophilic organic acid solvent, and the mole ratio of the o-nitrobenzene dimethyl sulfide to water during the chlorination reaction is 1:(5-15); a finished product of o-nitrobenzenesulfonyl chloride is obtained through refining and drying. Through HPLC detection, the content of the o-nitrobenzenesulfonyl chloride synthesized by means of the method is 98-98.5%; the yield is 0.72-0.75, the acquisition rate is 0.97 or above, the turbidity (ppm) is 1.5-2, and the melting point is 66-67 DEG C. By adopting the hydrophilic organic acid solvent, the problems about large-scale production discharging, yield and quality are solved, and meanwhile the purposes of mixed application and post-treatment separation of large-scale production water-soluble solvents are achieved.
Pharmaceutical intermediates in the synthesis of ortho-nitrophenyl-sulfonyl chloride (by machine translation)
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Paragraph 0013; 0016-0027, (2018/07/30)
This invention relates to pharmaceutical intermediates in the synthesis of ortho-nitrophenyl-sulfonyl chloride method, comprises the following steps: in the reaction container by adding 5 - hydroxy - 6 - methyl nitrobenzene - sulfur, potassium chloride solution, raising the temperature of the solution, the reaction, then batches and join the trichloro acetic acid solution, the stirring speed is; in time in three batches and adding lauryl carbonyl iron, in raised in temperature, to continue to reaction, the temperature is lowered, separating solid, filtering, for sodium sulfate solution many times, triethylamine solution many times, nonane solution many times, in the alcohol solution to recrystallize, desiccant dehydration, to get finished ortho-nitrophenyl-sulfonyl chloride. (by machine translation)
2-Nitrobenzenesulfonyl chloride and synthetic method and application thereof
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Paragraph 0006; 0021; 0022, (2017/08/30)
The invention discloses 2-nitrobenzenesulfonyl chloride and a synthetic method and application thereof; the synthetic method comprises the steps of (a) subjecting 2-nitrochlorobenzene and sodium thiomethoxide to etherification, filtering, recrystallizing the obtained filter cake, centrifugally separating, and drying to obtain dried 2-nitrophenyl sulfur ether; (b) chlorinating the dried 2-nitrophenyl sulfur ether to obtain a wet crude product; refining, and drying to obtain the finished 2-nitrobenzenesulfonyl chloride. By modifying the prior art, it is possible to eliminate the intermediate product, disulfides, with the turbidity of the product fully controlled to 2 and below, and the requirement of liquid crystal materials for the turbidity is met; compared with the prior art, the 2-nitrobenzenesulfonyl chloride and the synthetic method and application thereof have the advantages that the process cost is low and the more applications of 2-nitrobenzenesulfonyl chloride are available in the field of liquid crystal materials and other fields.