Sulfuric Acid → HCID 86753028, compound

Participants

Reaction Steps

2.8 g of 17beta-acetoxy 3-ethoxy 17alpha-ethynyl 6-formyl 3,5-estradiene, 8.5 ml (abs) ethanol (3.03 vol), 7 ml dimethylformamide (2.5 vol), and 0.13 g sodium borohydride (0.046 p) are introduced under agitation and under a nitrogen atmosphere into a 50 ml three-necked flask. The reaction is stopped after agitation for 22 hours. The reaction medium is hydrolyzed by introducing a solution composed of 2.8 ml (1 vol) of 2N sulphuric acid, 6 ml (2.1 vol) DMF, and 6 ml (2.1 vol) (abs) ethanol over 10 minutes. 2.1 g (yield=84%) of a creamy white product is obtained. M.p.=157° C.

Provenance & Evidence