反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
PROCEDURE
实验过程
Method E. Reaction of oxalyl chloride (70 λL, 0.8 mmol) and benzoic acid 53 (200 mg, 0.54 mmol) with subsequent reaction with 3-pyridinylmethylamine (60 λL, 0.6 mmol) gave benzamide 54 (171 mg, 68%) as a white powder: mp (EtOAc) 178-181° C.; 1H NMR δ 9.19 (t, J=5.9Hz, 1 H, CONH), 8.57 (d, J=1.6Hz, 1 H, H-2″), 8.47 (dd, J=4.8, 1.5Hz, 1 H, H-6″), 7.97 (dd, J=6.7, 1.8Hz, 2 H, H-2 , H-6), 7.81 (dd, J=6.7, 1.8Hz, 2 H, H-3, H-5), 7.74 (ddd J=8.1, 2.1, 1.6Hz, 1 H, H-4″), 7.68 (s, 1 H, H-5′), 7.65 (dd, J=8.3, 1.7Hz, 2 H, H-2″, H-6″), 7.41 (br d, J=8.3Hz, 2 H, H-3″, H-5″), 7.36 (ddd, J=8.1, 4.8, 0.7Hz, 1 H, H-5″), 4.87 (s, 2 H, CH2SO2), 4.51 (d, J=5.9Hz, 2 H, CH2N), 2.40 (s, 3 H, CH3); 13C NMR δ 165.7, 165.5, 148.9, 148.1, 145.2, 144.3, 135.9, 135.3, 135.2, 135.0, 134.9, 129.5 (2), 128.2 (2), 128.1 (2), 125.9 (2), 123.4, 122.2, 57.0, 40.5, 21.0; MS m/z 464.8 (MH+, 100%). Anal. calcd for C24H21N3O3S2: C, 62.18; H, 4.57; N, 9.06. Found: C, 62.30; H, 4.55; N, 9.10%.