HCID 70538349, compound → HCID 56627596, compound

Participants

Reaction Steps

One gram of 17α-acetoxy-11β-benzoyloxy-1α,2α-methylene-4,6-pregnadiene-3,20-dione is dissolved in 10 ml of "Dowtherm" (filtered over A12O3). The solution is heated under a stream of nitrogen gas for 30 minutes to 285° C. After cooling, the mixture is diluted with hexane, introduced into a silica gel column, and the "Dowtherm" is eluted with hexane. The thus-prepared compound is now eluted with methylene chloride and a gradually increasing proportion of chloroform. The individual fractions are tested for content and purity by thin-layer chromatography. The fractions having the desired compound are combined, concentrated, and the residue is recrystallized from benzene, thus obtaining 700 mg of 11β-benzoyloxy-1α,2α-methylene-4,6,16-pregnatriene-3,20-dione (79% of theory), m.p. 227°-229° C.

Provenance & Evidence