反应详情

Ethylene glycol (20 ml.) and p-TSA (5 mg.) is added to 17β-hydroxy-17α-methyl-5α-androstan-3-one (sold by Steraloids, Inc., Wilton, N.H., 3.0 g.) in methylene chloride (20 ml.). The mixture is heated on a steam bath until most of the methylene chloride is removed. The remainder of the methylene chloride is removed on a rotary evaporator. The mixture is cooled and a small amount of a sodium bicarbonate solution and water are added and the mixture filtered. The filtered solids are washed and dried to give the title compound, NMR (CDCl3), 0.83, 0.84, 1.20 and 3.29δ.

1. customis removed
2. customThe remainder of the methylene chloride is removed on a rotary evaporator
3. temperatureThe mixture is cooled
4. additiona small amount of a sodium bicarbonate solution and water are added
5. filtrationthe mixture filtered
6. washThe filtered solids are washed
7. customdried