反应详情

A solution of 0.11 g (0.17 mmol) (R)-N-[6-(4-benzyl-2-methyl-piperazin-1-yl)-4-(4-fluoro-2-methyl-phenyl)-pyridin-3-yl]-2-(3,5-bis-trifluoromethyl-phenyl)-N-methyl-isobutyramide in 3 ml acetic acid was deoxygenated by three cycles of evacuation and flushing with argon. After addition of 0.02 g palladium on charcoal (10%) the reaction vessel was evacuated and filled with hydrogen gas. The reaction mixture was stirred at room temperature under an atmosphere of hydrogen for 3 h. The reaction mixture was filtered over decalite followed by washing with tert-butyl methyl ether. The filtrate was washed with a 2 M aqueous solution of sodium hydroxide. The aqueous layer was extracted with three portions of tert-butyl methyl ether. The combined organic layers were dried over sodium sulfate and concentrated in vacuo to give 98 mg (98%) of the crude title compound as an off-white solid, which was used in the next step without further purification. MS m/e (%): 597 (M+H+, 100)

1. customflushing with argon
2. additionAfter addition of 0.02 g palladium on charcoal (10%) the reaction vessel
3. customwas evacuated
4. additionfilled with hydrogen gas
5. filtrationThe reaction mixture was filtered over decalite
6. washby washing with tert-butyl methyl ether
7. washThe filtrate was washed with a 2 M aqueous solution of sodium hydroxide
8. extractionThe aqueous layer was extracted with three portions of tert-butyl methyl ether
9. dry with materialThe combined organic layers were dried over sodium sulfate
10. concentrationconcentrated in vacuo