反应详情

温度

0 °C

To a solution of the product of EXAMPLE 35 (50 mg, 0.109 mmol) in MeOH (1 mL) was added sodium borohydride (13 mg, 0.33 mmol) at 0° C. The mixture was stirred at 0° C. for 30 min, diluted with water, and extracted with EtOAc. The combined organic layers were dried over Na2SO4, and the solvent was removed under reduced pressure. The residue was purified by preparative TLC (5% MeOH/DCM) to give the title compound. LC-MS m/z=460.17 (M+1). 1H NMR (500 MHz, CDCl3) δ 8.85 (d, J=4.7 Hz, 2H), 7.91 (d, J=8.6 Hz, 2H), 7.43-7.37 (m, 5H), 7.32-7.27 (m, 3H), 6.67 (s, 1H), 4.83 (dd, J=10.2 Hz, J=3.6 Hz, 1H), 3.81-3.72 (m, 1H), 3.35 (d, J=11.4 Hz, 1H), 3.01 (d, J=11.8 Hz, 1H), 2.66-2.46 (m, 3H), 2.32-2.22 (m, 1H), 2.21-2.08 (m, 2H), 1.96-1.80 (m, 2H).

1. extractionextracted with EtOAc
2. dry with materialThe combined organic layers were dried over Na2SO4
3. customthe solvent was removed under reduced pressure
4. customThe residue was purified by preparative TLC (5% MeOH/DCM)