反应详情

A solution of 800 mg of 11α-hydroxy-7α-methylestr-4-ene-3,17-dione (F) in 8 ml of dichloromethane was mixed at 0° C. with 1.21 ml of hexachloroacetone and 764 mg of triphenylphosphine and stirred at room temperature for 4 hours. Then, it was diluted with dichloromethane, washed neutral, dried on sodium sulfate, concentrated by evaporation in a vacuum and chromatographed on silica gel with hexane/ethyl acetate. 430 mg of pure 11β-chloro-7α-methyl-estr-4-ene-3,17-dione (F′) with a melting point of 215.1° C. was obtained ([α]D20=+182.7° (c=0.5% in chloroform)).

1. washwashed neutral
2. customdried on sodium sulfate
3. concentrationconcentrated by evaporation in a vacuum
4. customchromatographed on silica gel with hexane/ethyl acetate