Oxalic Acid → HCID 11761638, compound

Participants

Reaction Steps

14 g of silica gel is suspended in 30 ml of methylene chloride, mixed with 1.4 ml of saturated oxalic acid solution and stirred for 15 more minutes. 4.67 g (10 mmol) of 3,3;17,17-bis-(ethylenedioxy)-11β-(4-methoxyphenyl)-5-estrene is added to this suspension and the reaction mixture is stirred at room temperature for 4 more hours. Then, it is suctioned off on a frit, the frit residue is rewashed with methanol/methylene chloride and the thus obtained filtrate is shaken out with saturated sodium bicarbonate solution. The organic phase is dried on sodium sulfate and concentrated by evaporation in a vacuum. The residue is chromatographed on silica gel with a mixture of ethyl acetate/hexane. 3.28 g of 3,3-(ethylenedioxy)-11β-(4-methoxyphenyl)-5-estren-17-one is obtained as white foam.

Provenance & Evidence