编辑: hgtbkwd | 2019-07-13 |
yield: (79 mg, 65%);
1H NMR (300 MHz, DMSO-d6): δ = 7.
43 (s, 1H), 7.45 C 7.63 (m, 9H), 7.85 C 7.98 (m, 7H), 8.03 (s, 3H);
13C NMR (75 MHz, DMSO-d6): ? = 128.4 (2CH2), 129.1 (2CH2), 132.1 (CH), 135.2 (C), 168.8 (CO);
GC-MS (EI,
70 eV): m/z (%) [M+]121 (81),
105 (100),
77 (95),
51 (40),
50 (23),
44 (10). 4-Methylbenzamide[1] ethyl acetate/hexane (2:1);
yield: (90 mg, 67%);
1H NMR (300 MHz, DMSO-d6): δ = 2.38 (s, 3H, CH3), 7.26 C 7.31 (m, 2H), 7.32 (s, 1H), 7.78 C 7.85 (m, 2H), 7.94 (s, 1H, NH2);
13C NMR (DMSO-d6): ? = 21.8 (CH3), 128.4 (2CH), 129.6 (2CH), 132.4 (C), 141.9 (C), 168.7 (CO);
GC-MS (EI,
70 eV): m/z (%)[M+]
135 (58),
119 (100),
91 (84),
89 (22),
65 (45),
44 (43). 4-Methoxybenzamide [1] ethyl acetate/hexane (2:1);
yield: (126 mg, 83%);
1H NMR (300 MHz, DMSO-d6): ? = 3.83 (s, 3H), 6.99-7.03 (m, 2H), 7.27 (s, 1H), 7.85-8.00 (m, 3H);
13C NMR (75 MHz, DMSO-d6): ? = 56.2 (OCH3), 114.3 (2CH), 127.4 (C), 130.3 (2CH), 162.5 (C), 168.5 (CO);
GC-MS (EI,
70 eV): m/z (%) [M+]
151 (51),
135 (100),
107 (11),
92 (17),
77 (24). 4-(Methylthio)benzamide [2] ethyl acetate;
yield: (90 mg, 54%);
1H NMR (400 MHz, DMSO-d6) δ = 3.30 (s, 3H), 7.70 (s, 1H), 8.02 C 8.09 (m, 2H), 8.09 C 8.19 (m, 2H), 8.26 (s, 1H);
13C NMR (100 MHz, DMSO-d6) δ = 44.2.3 (SCH3), 127.9 (2CH), 129.3 (2CH), 139.7 (C), 143.8 (C), 167.5 (CO);
GC-MS (EI,
70 eV): m/z (%)[M+]
167 (89),
151 (100),
108 (24),
82 (11),
69 (17),
45 (35)
44 (34). 3-Methoylbenzamide [3] ethyl acetate/hexane (2:1);
yield: (130 mg, 86%);
1H NMR (300 MHz, DMSO-d6): ? = 3.83 (s, 3H, OCH3), 7.11 (ddd, J = 8.1, 2.6, 1.0 Hz, 1H), 7.32 C 7.56 (m, 4H), 8.03 (s, 1H);
13C NMR (75 MHz, DMSO-d6) δ = 56.1 (OCH3), 113.6, 117.9, 120.6, 130.2 (CH), 136.6 (C), 160.0 (C), 168.58. (CO);
GC-MS (EI,
70 eV): m/z (%)[M+]
151 (86),
150 (18),
135 (100),
107 (47),
92 (48),
77 (56),
63 (48),
44 (46),
38 (14). 3,5-Dimethylbenzamide[4] ethyl acetate/hexane (2:1);
yield: (130 mg, 87%);
1H NMR (300 MHz, DMSO-d6): δ = 2.33 (S, 3H, CH3), 2.34 (s, 3H, CH3), 7.16-7.18 (m, 1H), 7.31 (s, 1H), 7.52-7.53 (m, 2H), 7.91 (s, 1H);
13C NMR (75 MHz, DMSO-d6): δ = 21.7 (CH3), 21.8 (CH3), 126.2 (2CH), 133.3 (C), 135.2 (CH), 138.1 (2C), 169.1 (CO);
GC-MS (EI,
70 eV): m/z (%) [M+]
149 (59),
133 (100),
105 (60),
103 (24),
77 (42),
44 (44). 4-(tert-Butyl)benzamide[1] ethyl acetate/hexane (2:1);
yield: (80 mg, 45%);
1H NMR (300 MHz, DMSO-d6): δ = 1.33 (S, 9H, CH3), 7.31 (s, 1H), 7.45- 7.52 (m, 2H), 7.80-7.87 (m, 2H), 7.94 (s, 1H);
13C NMR (75 MHz, DMSO-d6) δ = 31.8 (3CH3), 35.4 (CCH3), 125.8 (2CH), 128.2 (2CH), 132.4 (C), 154.8 (C), 168.7 (CO);
GC-MS (EI,
70 eV): m/z (%) [M+]
177 (17),
163 (11),
162 (100),
115 (14),
91 (42),
44 (26). 4-Trifluoromethylbenzamide [1] ethyl acetate/hexane (2:1);
yield: (110 mg, 58%);
1H NMR (300 MHz, DMSO-d6): δ = 7.68 (s, 1H), 7.86 (dt, J = 8.2, 0.7 Hz, 2H), 8.11 (dt, J = 8.2, 0.7 Hz, 2H), 8.25 (s, 1H);
13C NMR (75 MHz, DMSO-d6) δ = 124.8 (q, 1JCF3 = 272.2 Hz, CF3) 126.15 (q, 4JCF3, = 3.8 Hz, CH), 129.2 (CH), 132.08 (q, 3JCF3 = 32.0 Hz), 138.9 , 167.62 (CO);
19F NMR (282 MHz, DMSO-d6);
δ = -61.03 (F). GC-MS (EI,
70 eV): m/z (%) [M+]
189 (61),
173 (100),
145 (98),
95 (15),
75 (14). NH2 O NH2 O F3C NH2 O NH2 O MeO NH2 O S NH2 O MeO NH2 O NH2 O Nicotinamide[1] ethyl acetate;
yield: (112 mg, 92%);