Methanesulfonic Acid → HCID 24768595, compound

Participants

Reaction Steps

To 251 mg of N-(1-Benzyloxy-6-morpholin-4-ylmethyl-2-oxo-2,3,4,7-tetrahydro-1H-azepin-3-(R)-yl)-4-(4-chloro-phenoxy)-benzenesulfonamide was added 8 mL of methanesulfonic acid. The reaction was stirred at room temperature for 20 hours, and then the solution was poured over ice. After the ice melted, the aqueous layer was extracted with ethyl ether. The aqueous layer was then neutralized with NaHCO3(s). The aqueous layers were then extracted with dichloromethane three times. The organic layers were then washed with NaCl(aq.) solution, and dried over Na2SO4(s). Filtration and solvent removal was followed by filtration over silica gel and elution with an ethyl acetate methanol mixture (4:1). Solvent removal, dilution with ethyl ether, filtration of the solids and drying gave 105 mg of a beige solid. MS: 1037 (2M+Na), 530 (M+Na), 508 (M+H).

Provenance & Evidence