反应详情

The procedure used for the preparation of 9a was repeated with 8g (145 mg, 0.242 mmol), Et3SiH (0.387 mL, 2.42 mmol), and trifluoroacetic acid (0.746 mL, 9.68 mmol) in dry ClCH2CH2Cl (6 mL) at 0° C. under nitrogen to give 9g (90.5 mg, 86%) as a white solid after crystallization from THF/CH2Cl2 /hexane. mp 165° C. (dec); IR (KBr) 3550-2550 (br), 3282, 1779, 1725, 1665, 1469, 1235 cm-1 ; 1H NMR (DMSO-d6) δ3.43-3.62 (2H, m), 3.76 (2H, s, CH2), 5.00 (1H, d, J=4.8 Hz), 5.67-5.73 (1H, m), 6.42 (3H, d, J=8.1 Hz), 7.07 (1H, t, J=8.1 Hz), 7.41 (1H, s), 9.11 (1H, d, J=8.2 Hz, NH), 12.17 (2H, br s, OH), 13.16 (1H, br s, CO2H); FDMS m/z 433 (M+), 434 (M+ +1); HRMS m/z Calcd for C18H16N3O6S2 (M+ +1): 434.0481, Found: 434.0448.