Diethyl Ether → HCID 70478952, compound

Participants

Reaction Steps

A mixture of 11β-difluoromethylestr-4-en-17-one (XII, Example 14, 0.9 g) in propynyl magnesium bromide (0.5M, 10 ml) and THF is kept at 20°-25° for 16 hours. Diethyl ether and aqueous ammonium chloride are added and the diethyl ether phase is separated and washed with water and concentrated to a solid. The solid is purified by chromatography through silica gel using ethyl acetate/hexane (20/80) as the irrigant. The appropriate fractions are pooled and concentrated to give the title compound, IR (mull) 3400, 2237 and 1666 cm-1 ; MS (m/e) 348, 330, 315, 266 and 251; NMR (CDCl3) 0.87, 1.86 and 6.0 δ.

Provenance & Evidence