反应详情

The hydrogenation vessel was charged with acetic acid (530 l), 3-oxo-4-aza-5-androstene-17β-carboxylic acid 2 (33.5 kg.), and ammonium acetate (1.0 kg, 0.1 eq.). After purging at 20-25° C. with nitrogen, the platinum oxide catalyst (3.0 kg.) was charged, the stirrer started and the temperature adjusted to 20-25° C. After purging with hydrogen, the stirring batch was allowed to take up hydrogen. After 30 minutes at ≦30° C., the temperature was adjusted to 60-65° C., and stirring continued until hydrogen uptake ceased. After purging with nitrogen, Solka Floc (1.7 kg.) was charged, and the hot reaction mixture recirculated through a filter until the solution was clear. The hot reaction filtrate was transferred to a clean vessel. The reactor was rinsed with hot acetic acid (100 l.), and the rinse was recirculated as a wash through the filter. The combined filtrates/wash were distilled under vacuum at ≦70° C. to about 3.6 volumes. The resulting slurry was cooled to ≦25° C. Methanol (130 l.) was added and the mixture stirred for at least 2 hours at ≦25° C. The product was collected by filtration; the cake washed with methanol and dried in vacuo at ≦60° C. Weight range: 25-28.5 kg (75-85% theory, 75-85% w/w).

1. customAfter purging at 20-25° C. with nitrogen
2. additionthe platinum oxide catalyst (3.0 kg.) was charged
3. customadjusted to 20-25° C
4. customAfter purging with hydrogen
5. customwas adjusted to 60-65° C.
6. customAfter purging with nitrogen, Solka Floc (1.7 kg.)
7. additionwas charged
8. filtrationa filter until the solution
9. customThe hot reaction filtrate was transferred to a clean vessel
10. washThe reactor was rinsed with hot acetic acid (100 l.)
11. washa wash through the filter
12. washThe combined filtrates/wash
13. distillationwere distilled under vacuum at ≦70° C. to about 3.6 volumes
14. temperatureThe resulting slurry was cooled to ≦25° C
15. additionMethanol (130 l.) was added
16. stirringthe mixture stirred for at least 2 hours at ≦25° C
17. filtrationThe product was collected by filtration
18. washthe cake washed with methanol
19. customdried in vacuo at ≦60° C