反应详情

To 2.25 gm. of sodium metal dissolved in 180 ml. of ethanol is added 8 ml. of β-phenylethyl mercaptan followed by 3 gm. of 17β-methanesulfonyloxy-1,4-androstadiene-3,11-dione. Heat the reaction at reflux for 48 hours. Obtain a residue in a manner similar to that described in Example 1A. Chromatograph the residue on a 300 gm. silica gel column eluting with chloroform/ethyl acetate (2:1). Combine the desired fractions as determined by thin layer chromatography, evaporate and crystallize the resultant residue from ether/hexane to obtain the title compound; m.p. 112°-115° C.

1. temperatureHeat
2. customthe reaction
3. temperatureat reflux for 48 hours
4. customObtain a residue in a manner similar to
5. washsilica gel column eluting with chloroform/ethyl acetate (2:1)
6. customevaporate
7. customcrystallize the resultant residue from ether/hexane