反应详情

2α-Fluoroandrostane-3,17-dione (315 mg) and 3-(R)-pyrrolidinyloxyamine dihydrochloride (Preparation 12, 190 mg) were dissolved in pyridine (5 ml) and stirred at RT for 1 h. After evaporation of the solvent, the crude reaction mixture was purified by flash chromatography (SiO2, CHCl3/MeOH/26% NH4OH 90/10/1). To the resulting oil obtained after fractions evaporation, dissolved in a 1/1 mixture of EtOAc/Et2O (20 ml) and cooled with an ice bath, an excess of 2N HCl solution in Et2O was added. The title compound I-bh was obtained, after filtration, as a white solid in 91% yield.

1. customAfter evaporation of the solvent
2. customthe crude reaction mixture
3. customwas purified by flash chromatography (SiO2, CHCl3/MeOH/26% NH4OH 90/10/1)
4. customTo the resulting oil obtained
5. customafter fractions evaporation
6. dissolutiondissolved in a 1/1 mixture of EtOAc/Et2O (20 ml)
7. temperaturecooled with an ice bath
8. additionan excess of 2N HCl solution in Et2O was added