Reference of 932-96-7, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 932-96-7 as follows.
General procedure:To a solution of 3-(chlorosulfonyl)benzoic acid (1.0 equiv, ca. 0.1 M) in dichloromethane, 4-bromo-N-methylaniline (3.1 equiv) was slowly added at 0 C with stirring. The mixture was stirred at room temp for 12 h. The solvent was removed with a nitrogen gas stream, the mixture was treated with 1 M NaOH (> 10 equiv), and was extracted with ether three times. The aqueous fraction was then acidified with 3 M HCl to pH ~1. The mixture turned cloudy during the addition. The resulting precipitate was collected by suction filtration on a Buchner funnel, washed with distilled water, and dried overnight at reduced pressure to give 3-(N-(4-bromophenyl)-N-methylsulfamoyl)benzoic acid (7a, 50-60%), which was used without further purification. To a solution of 7a (1.0 equiv, ca. 0.1 M), was added 4-chloro-N-methylaniline (1.1 equiv), EDCI (1.3 equiv), and DMAP (0.1 equiv). The mixture was stirred at room temp for 12 h and then diluted with excess EtOAc. The organic mixture was washed with 1 M aqueous HCl (2 times), 1 M aqueous NaHCO3 (2 times), and brine. The organic layer was dried over MgSO4, filtered, and concentrated in vacuo to yield a crude product, which was purified by silica gel column chromatography to give 3a as a thick gel.
According to the analysis of related databases, 932-96-7, the application of this compound in the production field has become more and more popular.
Reference:
Article; Choi, Soo Hyuk; Quinti, Luisa; Kazantsev, Aleksey G.; Silverman, Richard B.; Bioorganic and Medicinal Chemistry Letters; vol. 22; 8; (2012); p. 2789 – 2793;,
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