反应详情

The procedure used for the preparation of 9a was repeated with 8k (129 mg, 0.221 mmol), Et3SiH (0.353 mL, 2.21 mmol), and trifluoroacetic acid (0.681 mL, 8.84 mmol) in dry ClCH2CH2Cl (6 mL) at 0° C. under nitrogen to give 9k (79.1 mg, 86%) as a yellowish solid after crystallization from THF/CH2Cl2 /hexane. mp 170° C. (dec); IR (KBr) 3600-2800 (br), 3276, 1776, 1723, 1663 cm-1 ; 1H NMR (DMSO-d6) δ3.48 (1H, dd, J=18.9 and 6.0 Hz), 3.58 (1H, dd, J=18.9 and 2.5 Hz), 3.79 (2H, s, CH2), 5.00 (1H, d, J=5.0 Hz), 5.70 (1H, dd, J=8.1 and 5.0 Hz), 6.44 (1H, dd, J=6.0 and 2.5 Hz), 7.37 (1H, dd, J=8.1 and 4.2 Hz), 7.44 (1H, d, J=8.1 Hz), 7.58 (1H, s), 8.14 (1H, d, J=4.2 Hz), 9.15 (1H, d, J=8.1Hz, NH), 11.64 (1H, s, OH), 13.20 (1H, br s, CO2H); FDMS m/z 419 (M+ +1); Anal. Calcd for C17H14N4O5S2.(C4H8O) 0.17: C, 49.30; H, 3.59; N, 13.01. Found: C, 49.13; H, 3.38; N, 12.78.