反应详情

温度

45 °C

9.0 Kg of 17α-ethynyl-17β-hydroxy-6,16-dimethyleneandrost-4-en-3-one is added to a reactor vessel, flushed with nitrogen until the oxygen content is less than 4%. 108 Liters (85.3 Kg) of acetone is added and the solution heated to 45° C. A catalyst solution (prepared by the addition of 0.72 liters conc. sulfuric acid to 10.8 liters of deionized water, followed by the addition of 576 grams of mercuric oxide, red powder to the dilute acid) is added to the reaction mixture and stirred at 45° C. until the reaction is complete, as monitored by TLC. The reaction mixture is cooled to less than 25° C. and 2.3 Kg Celite 545, 2.2 Kg sodium acetate and 20 liters of water added and mixture stirred for 15 min. The resulting crude product is filtered using a pot filter coated with Celite 545. The reactor is rinsed with 50 liters of acetone and filtered. The combined filtrate is concentrated under vacuum to about 50 liters, cooled to below 20° C. and stirred for 15 min. The slurry is filtered and the filter cake washed with 10 liters of acetone and 20 liters of water. The filter cake is dried in a vacuum oven at 50° C. to yield 17α-acetyl-17β-hydroxy-6,16-dimethyleneandrost-4-en-3-one (mercury content 10,500 ppm).

1. customflushed with nitrogen until the oxygen content
2. addition108 Liters (85.3 Kg) of acetone is added
3. customA catalyst solution (prepared by the addition of 0.72 liters conc. sulfuric acid to 10.8 liters of deionized water
4. additionis added to the reaction mixture
5. temperatureThe reaction mixture is cooled to less than 25° C.
6. stirringmixture stirred for 15 min
7. filtrationThe resulting crude product is filtered
8. washThe reactor is rinsed with 50 liters of acetone
9. filtrationfiltered
10. concentrationThe combined filtrate is concentrated under vacuum to about 50 liters
11. temperaturecooled to below 20° C.
12. stirringstirred for 15 min
13. filtrationThe slurry is filtered
14. washthe filter cake washed with 10 liters of acetone and 20 liters of water
15. customThe filter cake is dried in a vacuum oven at 50° C.