反应详情

To a mixture of 0.178 g (0.1 mmol) of the product of Step A and 0.206 g (3.5 mmol) of n-propylamine dissolved in 10 mL of CH2Cl2 was added 0.5 g of finely powdered 4 Å molecular sieves. The reaction mixture was stirred under a nitrogen atmosphere at room temperature overnight, then 0.53 g (2.5 mmol) of sodium triacetoxyborohydride was added. The reaction was then stirred an addition 8 h at room temperature, then diluted with CH2Cl2 and MeOH. The mixture was filtered through a pad of Celite filter aid eluted with CH2Cl2, and the filtrate was washed with saturated aqueous NaHCO3. The organic layer was the separated, dried (Na2SO4), filtered and evaporated in vacuo. The residue was purified on a flash chromatography column eluted with CH2Cl2-MeOH—NH4OH (95:4:1) to afford the title compound.

1. additionwas added 0.5 g of finely powdered 4 Å molecular sieves
2. stirringThe reaction was then stirred
3. additionan addition 8 h at room temperature
4. filtrationThe mixture was filtered through a pad of Celite
5. filtrationfilter aid
6. washeluted with CH2Cl2
7. washthe filtrate was washed with saturated aqueous NaHCO3
8. dry with materialdried (Na2SO4)
9. filtrationfiltered
10. customevaporated in vacuo
11. customThe residue was purified on a flash chromatography column
12. washeluted with CH2Cl2-MeOH—NH4OH (95:4:1)