反应详情

The procedure used for the preparation of 9a was repeated with 8e (181 mg, 0.270 mmol), Et3SiH (0.431 mL, 2.70 mmol), and trifluoroacetic acid (0.832 mL, 10.8 mmol) in dry ClCH2CH2Cl (6 mL) at 0° C. under nitrogen to give 9e (120 mg, 88%) as a white solid after crystallization from EtOAc/CH2Cl2 /hexane. mp 145° C. (dec); IR (KBr) 3650-2500 (br), 1775, 1736, 1466, 1237 cm-1 ; 1H NMR (DMSO-d6) δ1.98 (3H, s, CH3), 3.43 (1H, d, J=18.1 Hz ), 3.58 (1H, d, J=18.1 Hz), 3.76 (2H, s, CH2), 4.64 (1H, d, J=12.8 Hz), 4.95 (1H, d, J=12.8 Hz), 5.05 (1H, d, J=5.0 Hz), 5.64-5.70 (1H, m), 6.42 (2H, d, J=8.0 Hz), 7.07 (1H, t, J=8.0 Hz), 7.41 (1H, s), 9.12 (1H, d, J=8.1 Hz, NH), 12.17 (2H, br s, OH), 13.60 (1H, br s, CO2H); FDMS m/z 505 (M+), 506 (M+ +1); Anal. Calcd for C21H19N3O8S2 : C, 49.89; H, 3.79; N 8.31. Found. C 50.15; H 3.79; N 8.60.