反应详情

The procedure used for the preparation of 5a was repeated with 4b (805 mg, 2.89 mmol) and 2N LiOH (5.1 mL) to provide 5b (680 mg, 94%) as a yellowish solid, which was recrystallized from THF/hexane. mp 210° C. (dec); IR (KBr) 3540-2500 (br), 3256 (br), 1688, 1461, 1230 cm-1 ; 1H NMR (DMSO-d6) δ 3.78 (2H, s, CH2), 6.42 (2H, d, J=8.1 Hz, Ar), 7.08 (1H, t, J=8.1 Hz, Ar), 7.46 (1H, s), 12.21 (2H, s, OH), 12.47 (1H, br s, CO2H); FDMS m/z 251 (M+), 252 (M+ +1); Anal. Calcd for C11H9NO4S: C, 52.58; H, 3.61; N, 5.57. Found: C, 52.36; H, 3.57; N, 5.38.