Dichloromethane → HCID 59750817, compound

Participants

Reaction Steps

Under a nitrogen atmosphere, N-methylmorpholine (51.0 μl, 0.465 mmol) and methanesulfonyl chloride (18.8 μl, 0.242 mmol) were added to a dichloromethane solution (4 ml) of the 4-[(4-chlorophenyl)sulfonyl]-4-(2,5-difluorophenyl)butylamine hydrochloride (80.0 mg, 0.202 mmol) obtained in Example 227. After stirring at room temperature for 15 hours, N-methylmorpholine (156 μl, 1.42 mmol) and methanesulfonyl chloride (10.0 μl, 0.129 mmol) were added. The resulting mixture was stirred at room temperature for 2 hours. After dilution with dichloromethane, the mixture was successively washed with a saturated aqueous solution of ammonium chloride, water, and brine, dried over magnesium sulfate and then, concentrated. The residue thus obtained was subjected to flash chromatography on a silica gel column, and the fraction obtained from the hexane:ethyl acetate=1:1 eluate was concentrated. The solid thus obtained was recrystallized from ethyl acetate-hexane, whereby the title compound (71.5 mg, 0.163 mmol, 81%) was obtained as colorless plate crystals.

Provenance & Evidence