反应详情

A solution of 1.24 g of 4'-chlorobiphenyl-4-carbonyl-[2(R)-hydroxy-2-phenylethyl]amide in 20 ml of pyridine is cooled in an ice bath and treated with a solution of 921 mg of methanesulfonic acid anhydride in dichloromethane. The reaction mixture is stirred for additional 16 hours at 5°, ethyl acetate and saturated aqueous sodium hydrogencarbonate are added, the organic layer is separated, dried and concentrated in vacuo. Vacuum flash chromatography on silica gel (toluene/ethyl acetate =3/1) yields the compound as pale yellow crystals; m.p.: 121.5° (recrystallized from ethanol); [α]D20 =+133.5° (c=1.3, methanol);

1. customthe organic layer is separated
2. customdried
3. concentrationconcentrated in vacuo