反应详情

To a stirred solution of phenylenediamine (6.93 g, 64.08 mmol) in CH3CN was added pyridine (6.05 g, 76.89 mmol). After stirring at room temperature for 10 minutes it was cooled to ˜10° C. and added phenylmethylsulfonyl chloride (6 g, 32.04 mmol). Reaction was further stirred for 14 hours at ambient temperature. Reaction was quenched with aqueous NaHCO3 (saturated) and stirred for 30 minutes. Solid was filtered, and dried under high vacuum to obtain crude N-(3-aminophenyl)-1-phenylmethanesulfonamide 26 (3.1 g, 19% yield). MS (ES) m/z 263 (M+H+).

1. temperaturewas cooled to ˜10° C.
2. customReaction
3. stirringwas further stirred for 14 hours at ambient temperature
4. customReaction
5. customwas quenched with aqueous NaHCO3 (saturated)
6. stirringstirred for 30 minutes
7. filtrationSolid was filtered
8. customdried under high vacuum