反应详情

The procedure used for the preparation of 9a was repeated with 8h (169 mg, 0.276 mmol), Et3SiH (0.441 mL, 2.76 mmol), and trifluoroacetic acid (0.849 mL, 11.0 mmol) in dry ClCH2CH2Cl (6 mL) at 0° C. under nitrogen to give 9h (121 mg, 98%) as a white solid after crystallization from THF/hexane. mp 155° C. (dec); IR (KBr) 3500-2500 (br), 1768, 1670, 1467 cm-1 ; 1H NMR (DMSO-d6) δ1.97 (3H, s, CH3), 3.31 (1H, d, J=18.0 Hz), 3.51 (1H, d, J=18.0 Hz), 3.76 (2H, s, CH2), 5.00 (1H, d, J=4.5 Hz), 5.57 (1H, dd, J=8.0 and 4.5 Hz), 6.42 (2H, d, J=8.1 Hz), 7.07 (1H, t, J=8.1 Hz), 7.41 (1H, s), 9.07 (1H, d, J=8.0 Hz, NH), 12.20 (2H, br s, OH), 13.20 (1H, br s, CO2H); FDMS m/z 448 (M+ +1); HRMS m/z Calcd for C19H18N3O6S2 (M+ +1): 448.0637, Found: 448.0607.