ChemicalBook CAS DataBase List 2-Nitrobenzenesulfonyl chloride

2-Nitrobenzenesulfonyl chloride synthesis

11synthesis methods

Product Name:2-Nitrobenzenesulfonyl chloride
CAS Number:1694-92-4
Molecular formula:C6H4ClNO4S
Molecular Weight:221.62

2-Nitrobenzenesulfonyl chloride is isolated as an intermediate in the production of 2-nitrobenzenesulfonic acid. When 2,2' - dinitrodiphenyl disulfide is chlorinated in an organic solvent the product is 2-nitrophenylsulfenyl chloride.

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Yield:1694-92-4 97.5%

Reaction Conditions:

with formic acid;chlorine at 40; for 3 h;Temperature;

Steps:

2.3; 2.4; 2.5; 3.3; 3.4; 3.5
The o-nitrophenyl sulfide produced by the second etherification of steps (1) and (2) is subjected to chlorination reaction in 4 times.The formic acid is added as a hydrophilic organic acid solvent, and the chlorination reaction conditions are as follows:The reaction was carried out at 40 ° C for 3 hours.The degree of vacuum is 50mmH2O,The amount of chlorine gas introduced is stopped after the reaction system is cooled down;(4) Refining is carried out in five steps using a reaction vessel in which the wet crude product which has been subjected to the chlorination reaction and dissolved in toluene is dissolved in toluene at 40-50 ° C, and then slowly cooled to 5 ° C. Filtering; the weight ratio of the dried wet crude to toluene is 1.75:1;(5) Finally, vacuum drying to obtain o-nitrobenzenesulfonyl chloride, the yield is 97.5%, the HPLC content is 98.8%, the turbidity is 1.4 ppm, and the liquid crystal clarity can be improved by 3.8%.

References:

Suzhou Zechen Trade Co., Ltd.;Bao Renkang;Ding Bo CN110105251, 2019, A Location in patent:Paragraph 0052; 0056-0058; 0059; 0063-0065

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