反应详情

To a solution of N-[(3RS,4SR)-4-(3,4-dichloro-phenyl)-1-(piperidine-4-carbonyl)-pyrrolidin-3-yl]-4-methoxy-N-methyl-3-trifluoromethyl-benzamide (50 mg, 0.90 mmol) in acetone (0.5 mL) was added potassium carbonate (finely milled) (19 mg, 0.13 mmol), ethanesulfonyl chloride (13 μL, 0.13 mmol) and acetone (0.5 mL). The suspension was stirred for 18 h at ambient temperature. It was diluted with ethyl acetatec (10 mL) and washed with an aqueous solution of Na2CO3 (1 M, 10 mL) and brine (10 mL). The aqueous layers were extracted with ethyl acetate (10 mL) and the combined organic layers were dried over sodium sulfate. Purification by chromatography (SiO2, heptane:ethyl acetate=30:70 to 0:100) afforded the title compound (44 mg, 76%) as an off-white foam. MS m/e: 650.2 [M]+.

1. additionIt was diluted with ethyl acetatec (10 mL)
2. washwashed with an aqueous solution of Na2CO3 (1 M, 10 mL) and brine (10 mL)
3. extractionThe aqueous layers were extracted with ethyl acetate (10 mL)
4. dry with materialthe combined organic layers were dried over sodium sulfate
5. customPurification by chromatography (SiO2, heptane:ethyl acetate=30:70 to 0:100)