Sodium methanethiolate → HCID 86748620, compound

Participants

Reaction Steps

130 g of the compound prepared in Example 1 c) are dissolved in 1.4 l of absolute dimethylformamide, 7.81 g of sodium methanethiolate are added and the reaction mixture is heated under reflux for 3 hours. The mixture is cooled and then poured onto water and the aqueous phase is extracted with ethyl acetate. The combined organic phases are washed repeatedly with saturated sodium chloride solution, dried over sodium sulphate and concentrated in vacuo. The residue is chromatographed on silica gel with a mixture of ethyl acetate/hexane and 76.9 g of 3,3;17,17-Bis-(ethylenedioxy)-11β-(4-hydroxyphenyl)-5-oestrene are obtained in the form of a white foam.

Provenance & Evidence