反应详情

A solution of Intermediate 153c (1.21 g, 2.1 mmol) in ethanol (IMS grade, 20 mL) was treated with water (1 mL) and ammonium formate (1.33 g, 21 mmol). The mixture was purged with N2 then 10% Pd/C (0.67 g, 0.63 mmol Pd) was added. The mixture was heated to reflux for 1 h then filtered through celite and the filtrate was concentrated in vacuo. The residue was partitioned between EtOAc and water. The phases were separated and the aqueous layer was extracted with EtOAc (×2). The combined organic phase was washed with brine, dried (Na2SO4) and concentrated in vacuo. The residue was purified by FCC, using 0-40% EtOAc in cyclohexane, to give the title compound (0.53 g, 41% over 2 steps) as a golden gum. LCMS (Method 3): Rt 4.55 min, nth 486.5

1. customThe mixture was purged with N2
2. temperatureThe mixture was heated
3. temperatureto reflux for 1 h
4. filtrationthen filtered through celite
5. concentrationthe filtrate was concentrated in vacuo
6. customThe residue was partitioned between EtOAc and water
7. customThe phases were separated
8. extractionthe aqueous layer was extracted with EtOAc (×2)
9. washThe combined organic phase was washed with brine
10. dry with materialdried (Na2SO4)
11. concentrationconcentrated in vacuo
12. customThe residue was purified by FCC