反应详情

To a solution of 2-methoxy-N-(4-(4-nitronaphthalen-1-yloxy)pyridin-2-yl)acetamide (50.0 g, 142 mmol) in DMF (500 mL) under nitrogen was added palladium on carbon (10% w/w Pd/C, 5.0 g, 14.15 mmol) and the mixture was purged with hydrogen and maintained under a slight positive hydrogen atmosphere for 48 hr. The catalyst was removed by filtration through celite and the pad washed with DMF (2×100 mL) and then DCM (100 mL). The solvents were removed in vacuo to afford a dark brown residue which was treated with water (150 mL) and the mixture evaporated. Toluene (100 mL) was added and evaporated to remove residual water. After drying overnight under vacuum, the material was triturated from diethyl ether (250 mL) to give the title compound, Intermediate B1, as a green solid (43.3 g, 85%): m/z 324 (M+H)+ (ES+).

1. customthe mixture was purged with hydrogen
2. temperaturemaintained under a slight positive hydrogen atmosphere for 48 hr
3. customThe catalyst was removed by filtration through celite
4. washthe pad washed with DMF (2×100 mL)
5. customThe solvents were removed in vacuo
6. customto afford a dark brown residue which
7. customthe mixture evaporated
8. additionToluene (100 mL) was added
9. customevaporated
10. customto remove residual water
11. customAfter drying overnight under vacuum
12. customthe material was triturated from diethyl ether (250 mL)