反应详情

To a solution of 9 (2.81 g, 7.74 mmol) in TFA (30 ml) was added dropwise Et3SiH (7.42 ml, 46.44 mmol) at 0° C. Stirring was continued at 0° C. for 2 hours. Then, the solvent was evaporated, and the residue was purified by chromatography, CombiFlash silica gel column, hexane/CH2Cl2, CH2Cl2 from 0% to 50%, to give compound 10 as a clear oil (mixture of cis and trans diastereomers, 2.63 g, 97%). 1H NMR (CDCl3) δ 1.18-1.34 (m, 3H), 1.88 (dd, J=25.2 Hz, 12.4 Hz) and 2.14-2.19 (m, total 1H), 2.25-2.33 (m) and 2.43-2.55 (m, total 1H), 2.67-2.74 (m) and 2.82-2.92 (m, total 1H), 3.00-3.18 (m, 2H), 4.08-4.29 (m, 3H), 6.72-7.42 (m, 7H).

1. customThen, the solvent was evaporated
2. customthe residue was purified by chromatography, CombiFlash silica gel column, hexane/CH2Cl2, CH2Cl2 from 0% to 50%