Acetic Anhydride → HCID 86738163, compound

Participants

Reaction Steps

200 mg of 17α-ethynyl-1α,17-dihydroxy-18-methyl-4,15-estradien-3-one is dissolved in 10 ml of pyridine and combined under ice-cooling dropwise with 3 m of acetic anhydride. The solution is then allowed to warm up and agitated at room temperature overnight. Thereafter the reaction mixture is stirred into ice water, the precipitated, oily-crystalline product is vacuum-filtered, taken up in ethyl acetate, washed neutral, dried over Na2SO4, and concentrated to dryness under vacuum. The remaining residue is crystallized from ether/hexane, thus obtaining 165 mg of 1α-acetoxy-17α-ethynyl-17-hydroxy-18-methyl-4,15-estradien-3-one, mp 123°-126° C.

Provenance & Evidence