HCID 13960166, compound → HCID 13960169, compound

Participants

Reaction Steps

9.3 mg of 24,24-difluoro-3β,25-dihydroxy-26,27-dimethylcholesta-5,7-diene was dissolved in a mixture of 90 ml of benzene and 40 ml of ethanol, and in anargon stream at 0° C., the solution was irradiated with ultra-violetlight for 7 minutes using a medium-pressure mercury lamp through a Vycor filter. Subsequently, the reaction mixture was heated under reflux for 1 hour in at atmosphere of argon. The solvent was evaporated under reduced pressure, and the resulting crude product was purified by thin-layer silica gel chromatography (developing solvent: benzene/ethyl acetate=10:1;developed four times) to give 2.6 mg of the captioned vitamin D3 derivative [the compound of formula (I) in which X is H].

Provenance & Evidence