反应详情

To a solution of the product of Step B (0.06 g; 0.172 mmol) in 1M BH3 in THF (0.35 ml; 0.35 mmol) CF3CO2H (0.4 ml) was added drop wise at 0° C. with stirring. After the addition was completed (˜5 min) the reaction was quenched with H2O (0.5 ml) and solvents were removed under reduced pressure. The residue was diluted to 10 ml with EtOAc and was washed with 10% NaOH (2×2 ml), brine and dried over anhydrous MgSO4 and filtered. The filtrate was evaporated to dryness under reduced pressure to give the title compound (0.026 g; 43%) as a creamy foam, which was used in the next step without further purification. 1H-NMR (CDCl3) 1.49 (m, 6H); 1.7 (broad s, 1H+H2O); 3.45 (tr, 2H, J=8.9 Hz); 3.65 (tr, 2H, J=8.9 Hz); 4.19 (m, 4H); 6.75 (d, 1H, J=7.7 Hz); 6.97 (d, 1H, J=8.5 Hz); 7.17 (tr, 1H, J=7.7); 7.52 (d, 1H, J=7.2 Hz); 7.68 (d, 1H, J=1.9 Hz); 7.78 (dd, 1H, J=1.9, 7.2 Hz).

1. additionAfter the addition
2. custom(˜5 min)
3. customwas quenched with H2O (0.5 ml) and solvents
4. customwere removed under reduced pressure
5. additionThe residue was diluted to 10 ml with EtOAc
6. washwas washed with 10% NaOH (2×2 ml), brine
7. dry with materialdried over anhydrous MgSO4
8. filtrationfiltered
9. customThe filtrate was evaporated to dryness under reduced pressure