反应详情

The procedure used for the preparation of 9a was repeated with 8j (186 mg, 0.301 mmol), Et3SiH (0.480 mL, 3.01 mmol), and trifluoroacetic acid (0.927 mL, 12.0 mmol) in dry ClCH2CH2Cl (6 mL) at 0° C. under nitrogen to give 9j (123 mg, 90%) a s a brownish solid after crystallization from THF/CH2Cl2 /hexane. mp 175° C. (dec); IR (KBr) 3600-2700 (br), 3277, 1780, 1730, 1663 cm-1 ; 1H NMR (DMSO-d6) δ3.63 (1H, d, J=18.0 Hz), 3.78 (2H, s, CH2), 3.98 (1H, d, J=18.0 Hz), 5.15 (1H, d, J=4.8 Hz), 5.69 (1H, dd, J=8.1 and 4.8 Hz), 7.37 (1H, dd, J=8.4 and 4.3 Hz), 7.44 (1H, dd, J=8.4 and 1.1 Hz), 7.58 (1H, s), 8.14 (1H, dd, J=4.3 and 1.1 Hz), 9.23 (1H, d, J=8.1 Hz, NH), 11.62 (1H, s, OH), 13.80 (1H, br s, CO2H); FDMS m/z 453 (M+ +1, 35Cl), 455 (M+ +1, 37Cl); HRMS m/z Calcd for C17H1435ClN4O5S2 (M+ +1): 453.0094, Found: 453.0090.