反应详情

Yield: 50%; off-white solid; recrist. solvt.: EtOH; TLC: Rf=0.43 (EtOAc/EtOH 9/1); RPTLC: Rf=0.43 (AcOH/H2O 8/2); mp=136° C.; IR (υ cm−1): 1730 (CO); NMR (DMSO-d6) δ (ppm): 7.79 (s, 2H, ArH), 7.14 (s, 2H, ArH), 4.06-4.02 (m, 2H, CH2), 3.93-3.89 (q, J 7.0 Hz, 2H, CH2), 3.59-3.56 (t, J=7.0 Hz, 1H, CH), 2.80-2.77 (m, 2H, CH2), 1.88 (br, 1H, NH), 1.41-1.39 (t, J=7.0 Hz, 3H, CH3), 1.15-1.12 (t, J=7.0 Hz, 3H, CH3); MS (ESI+) m/z 911.7 [(M+DMSO)+, 100], 833.7 [(M+H)+, 75]; Anal. Calcd. for C19H19I4NO4: C, 27.40; H 2.30; N, 1.68. Found: C, 27.54; H, 1.94; N, 1.66. Solubility 10−3 M in water after preparing a solution at 10−1 M in DMSO. It is noteworthy that if a suspension of L-T4 is prepared overnight, the yield can be increased.

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