Lithium Carbonate → Atamestane

関与物質

反応手順

147.78 mg (2 mmol) of lithium carbonate is heated to 130° C. in 3 ml of N-methyl-pyrrolidone under nitrogen atmosphere. 426 mg (1 mmol) of 2α-iodo-1α-methyl-androst-4-ene-3,17-dione of example 3 is added to this preheated solution. The solution is stirred for another 2 hours at this temperature. After cooling to room temperature, the solution is added in 20 ml of ice water and the product is extracted with ethyl acetate. After evaporation of the solvent, the crude product is purified with ethyl acetate/hexane as mobile solvent by chromatography on silica gel. Concentration by evaporation of the fractions and recrystallization from ethyl acetate yields 178 mg (60% of theory) of 1-methylandrosta-1,4-diene-3,17-dione of melting point 169° C.

情報源と証拠