反应详情

To 2.462 kg. of methyl 4-androsten-3-one-17β-carboxylate in 24.6 l of methanol was added 1.23 kg. of potassium hydroxide in 4.9 l. of water. The reaction mixture was refluxed under nitrogen for 6 hours, and then allowed to cool to room temperature overnight. The mixture was acidified with 3200 ml. of 6 N hydrochloric acid. Most of the product crystallized as fine crystals. Then, 14 l. of water was added in a stream over 30 minutes, which precipitated all of the product. The mixture was aged with stirring for 4 hours at 30° C. The mixture was filtered on a cap funnel and washed with water until the wash water showed neutral. The product was dried in an oven at 50° C. overnight. The product, having a m.p. of 245°-248° C., was obtained in 98% yield (2.313 g.).

1. temperatureThe reaction mixture was refluxed under nitrogen for 6 hours
2. customMost of the product crystallized as fine crystals
3. additionof water was added in a stream over 30 minutes
4. customwhich precipitated all of the product
5. filtrationThe mixture was filtered on a cap funnel
6. washwashed with water until the wash water showed neutral
7. customThe product was dried in an oven at 50° C. overnight
8. customwas obtained in 98% yield (2.313 g.)