HRID1526816

反应详情

EQUATION

反应方程式

HRID 1526816 的结构方程式

PROCEDURE

实验过程

Method E. Reaction of oxalyl chloride (102 λL, 1.17 mmol) and benzoic acid 17 (280 mg, 0.78 mmol) with subsequent coupling to 3-pyridinylmethylamine (87 λL, 0.86 mmol) gave benzamide 18 (169 mg, 48%) as a white powder: mp (EtOAc) 196-198° C.; 1H NMR δ 9.20 (t, J=5.9 Hz, 1 H, CONH), 8.57 (br s, 1 H, H-2′), 8.46 (br s, 1 H, H-6′), 8.00 (br dd, J=8.6, 1.8Hz, 2 H, H-2, H-6), 7.89 (br dd, J=8.6, 1.8Hz, 2 H, H-3, H-5), 7.80 (br d, J=8.5Hz, 2 H, H-2″, H-6″), 7.71-7.76 (m, 2 H, H-4′, H-4″), 7.62 (br dd, J=8.2, 7.5 Hz, 2 H, H-3″, H-5″), 7.36 (dd, J=7.8, 4.8Hz, 1 H, H-5′), 4.68 (s, 2 H, CH2SO2), 4.50 (d, J=5.8Hz, 2 H, CH2N), 2.13 (s, 3 H, CH3); 13C NMR δ 165.4, 157.9, 149.9, 148.8, 148.0, 138.3, 135.3, 135.0, 134.8, 133.8, 129.1 (2), 128.7, 128.1 (2), 128.0 (2), 125.8, 125.3 (2), 123.4, 52.7, 40.4, 9.5; MS m/z 448.5 (MH+, 100%). Anal. calcd for C24H21N3O4S: C, 64.41; H, 4.73; N, 9.39. Found: C, 64.23; H, 4.71; N, 9.37%.