反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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%.