编辑: hgtbkwd | 2019-07-13 |
1H NMR (300 MHz, DMSO-d6): ? = 7.52-7.55 (m, 1H), 7.66 (s, 1H), 8.03 C 8.51 (m, 2H), 8.76 (s, 1H), 9.10 (s, 1H). 13CNMR (DMSO-d6): ? =124.5 (CH), 130.7 (C), 136.1 (CH), 149.6 (CH), 152.8 (CH), 163.7 (CO);
GC-MS (EI,
70 eV): m/z (%)[M+]
122 (100),
106 (60),
78 (75),
51 (36),
50 (18),
44 (10). Isonicotinamide [1] ethyl acetate;
yield: (115 mg, 94%);
1H NMR (400 MHz, DMSO-d6) δ = 7.76 (s, 1H), 7.73 C 7.89 (m, 2H), 8.29 (s, 1H), 8.47 C 8.89 (m, 2H);
13C NMR (100 MHz, DMSO-d6) δ = 122.3 (2CH), 142.2 (C), 151.1 (2CH), 167.3 (CO);
GC-MS (EI,
70 eV): m/z (%)[M+]
122 (100),
106 (43),
79 (11),
78 (56),
50 (19),
44 (11). Thiophene-2-carboxamide. [1] ethyl acetate;
yield: (60 mg, 47%);
1H NMR (300 MHz, DMSO-d6) δ = 7.16 (dd, J = 4.9, 3.7 Hz, 1H), 7.42 (s, 1H), 7.51 C 7.92 (m, 2H), 8.00 (s, 1H).;
13CNMR (75 MHz, DMSO-d6): δ = 128. (CH), 129.5 (CH), 131.8 (CH), 141.2 (C), 163.7 (CO). GC-MS (EI,
70 eV): m/z (%) [M+]
127 (51),
111 (100),
83 (13),
58 (10),
39 (36). Quinoline-3-carboxamide [5] ethyl acetate;
yield: (168 mg, 97%);
1H NMR (300 MHz, DMSO-d6) δ = 7.74 (ddd, J = 8.0, 6.9, 1.2 Hz, 2H), 7.91 (ddd, J = 8.4, 6.9, 1.5 Hz, 1H), 8.00 C 8.19 (m, 2H), 8.37 (s, 1H), 8.91 (d, J = 2.2 Hz, 1H), 9.36 (d, J = 2.2 Hz, 1H);
13CNMR (75 MHz, DMSO-d6);
δ = 127.5 (CH), 127.7 (C), 128.3 (CH), 129.5 (CH), 130.0 (C), 132.1 (CH), 136.8 (CH), 149.2 (CH), 149.9 (C), 167.3 (CO);
GC-MS (EI,
70 eV): m/z (%)[M+]
172 (85),
156 (69),
155 (20),
129 (12),
128 (100),
127 (19),
101 (54),
75 (37),
44 (40). 2-Naphthamide [2] ethyl acetate/hexane (2:1);
yield: (60 mg, 35%);
1H NMR (300 MHz, DMSO-d6): ? = 7.54 (s, 1H), 7.57-7.70 (m, 2H), 7.93-8.10 (m, 4H), 8.20 (s, 1H), 8.54 (s, 1H);
13CNMR (DMSO-d6): ? = 125.3, 127.5, 128.5, 128.7, 129.8, 132.5, 133.1 135.1, 168.9 (CO);
GC-MS (EI,
70 eV): m/z (%)[M+]
171 (80),
156 (12),
155 (99),
127 (100),
75 (10). 1-Naphthamide [1] ethyl acetate/hexane (2:1);
yield: (100 mg, 58%);
1H NMR (300 MHz, DMSO-d6): ? = 7.49-7.78 (m, 5H), 7.99-8.06 (m, 3H), 8.32-8.42 (m, 1H);
13C NMR (DMSO-d6): ? = 125.8, 126.0, 126.5, 127.0, 127.5, 129.1, 130.6 (CH), 130.7, 134.1, 135.5 (C), 171.5 (CO);
GC-MS (EI,
70 eV): m/z (%)[M+]
171 (86),
170 (31),
156 (9),
155 (82),
127 (100),
126 (25)
77 (11). 6-Methoxy-2-naphthamide[6] ethyl acetate/hexane (2:1);
yield: (70 mg, 35%);
1H NMR (300 MHz, DMSO-d6): 1H NMR (300 MHz, DMSO- d6) δ = 3.93 (s, 3H, OCH3), 7.26 (dd, J = 8.9, 2.5 Hz, 1H........