反应详情

Add 3-{1-[4-(4-acetyl-3-hydroxy-2-propyl-phenoxymethyl)-phenyl]-vinyl}-benzonitrile (0.105 g, 0.255 mmol), ethyl acetate (50 ml) and PtO2 (0.010 g) to a Parr pressure vessel. Purge the reaction vessel with nitrogen, pressurize the reaction mixture with hydrogen (400 KPa), seal the vessel and agitate the reaction at ambient temperature. Continue the reaction for 2.5 hours. Vent the excess hydrogen from the vessel and purge the vessel with nitrogen. Filter the reaction mixture to remove the platinum catalyst. Add the filtrate and PtO2 (0.019 g) to a Parr pressure vessel. Purge the reaction vessel with nitrogen, pressurize the reaction mixture with hydrogen (400 KPa), seal the vessel and agitate the reaction at ambient temperature. Continue the reaction for 6 hours. Vent the excess hydrogen from the vessel and purge the vessel with nitrogen. Filter the reaction mixture to remove the platinum catalyst and remove the solvent under vacuum. Add the concentrate, ethyl acetate (50 ml) and PtO2 (0.022 g) to a Parr pressure vessel. Purge the reaction vessel with nitrogen, pressurize the reaction mixture with hydrogen (400 KPa), seal the vessel and agitate the reaction at ambient temperature. Continue the reaction for 18 hours. Vent the excess hydrogen from the vessel and purge the vessel with nitrogen. Filter the reaction mixture to remove the platinum catalyst and remove the solvent under vacuum. Add the concentrate, ethyl acetate (150 ml), Pt catalyst from previous filtrations and PtO2 (0.105 g) to a Parr pressure vessel. Purge the reaction vessel with nitrogen, pressurize the reaction mixture with hydrogen (400 KPa), seal the vessel and agitate the reaction at ambient temperature. Continue the reaction for 22.5 hours. Vent the excess hydrogen from the vessel and purge the vessel with nitrogen. Filter the reaction mixture to remove the platinum catalyst. The mixture is filtered and concentrated to give 25 mg, 25%, as a film. LCMS M−1 412.

1. customPurge the reaction vessel with nitrogen
2. customseal the vessel
3. customthe reaction at ambient temperature
4. customthe reaction for 2.5 hours
5. customVent the excess hydrogen from the vessel and purge the vessel with nitrogen
6. filtrationFilter the reaction mixture
7. customto remove the platinum catalyst
8. additionAdd the filtrate and PtO2 (0.019 g) to a Parr pressure vessel
9. customPurge the reaction vessel with nitrogen
10. customseal the vessel
11. stirringagitate
12. customthe reaction at ambient temperature
13. customthe reaction for 6 hours
14. customVent the excess hydrogen from the vessel and purge the vessel with nitrogen
15. filtrationFilter the reaction mixture
16. customto remove the platinum catalyst
17. customremove the solvent under vacuum
18. additionAdd the concentrate, ethyl acetate (50 ml) and PtO2 (0.022 g) to a Parr pressure vessel
19. customPurge the reaction vessel with nitrogen
20. customseal the vessel
21. stirringagitate
22. customthe reaction at ambient temperature
23. customthe reaction for 18 hours
24. customVent the excess hydrogen from the vessel and purge the vessel with nitrogen
25. filtrationFilter the reaction mixture
26. customto remove the platinum catalyst
27. customremove the solvent under vacuum
28. additionAdd the concentrate, ethyl acetate (150 ml), Pt catalyst
29. filtrationfrom previous filtrations and PtO2 (0.105 g) to a Parr pressure vessel
30. customPurge the reaction vessel with nitrogen
31. customseal the vessel
32. stirringagitate
33. customthe reaction at ambient temperature
34. customthe reaction for 22.5 hours
35. customVent the excess hydrogen from the vessel and purge the vessel with nitrogen
36. filtrationFilter the reaction mixture
37. customto remove the platinum catalyst
38. filtrationThe mixture is filtered
39. concentrationconcentrated
40. customto give 25 mg, 25%