Hydrochloric Acid → HCID 16662044、化合物

反応式

[CH3:1][C:2]1([CH3:35])[C:8](=[O:9])[NH:7][C:6]2[N:10]=[CH:11][C:12](/[CH:14]=[CH:15]/[C:16]([N:18]([CH3:34])[CH2:19][C:20]3[CH:25]=[CH:24][CH:23]=[C:22]([O:26][C:27]([F:30])([F:29])[F:28])[C:21]=3[O:31][CH2:32][CH3:33])=[O:17])=[CH:13][C:5]=2[CH2:4][NH:3]1.[ClH:36]>C(Cl)Cl.C(OCC)C>[ClH:36].[CH3:35][C:2]1([CH3:1])[C:8](=[O:9])[NH:7][C:6]2[N:10]=[CH:11][C:12](/[CH:14]=[CH:15]/[C:16]([N:18]([CH3:34])[CH2:19][C:20]3[CH:25]=[CH:24][CH:23]=[C:22]([O:26][C:27]([F:29])([F:30])[F:28])[C:21]=3[O:31][CH2:32][CH3:33])=[O:17])=[CH:13][C:5]=2[CH2:4][NH:3]1

参加物

実験手順

A stirring solution of (E)-3-(3,3-dimethyl-2-oxo-2,3,4,5-tetrahydro-1H-pyrido[2,3-e][1,4]diazepin-7-yl)-N-methyl-N-(2-ethoxy-3-trifluoromethoxybenzyl)acrylamide (0.172 g, 0.349 mmol) in CH2Cl2 (4 mL) under N2 was treated with anhydrous HCl (0.17 mL of a 2 M solution in diethyl ether, 0.34 mmol). After stirring for 18 h, the resulting solid was collected by filtration, washed with Et2O (100 mL) and dried to yield the title compound (0.11 g, 62%) as an off white solid and as a mixture of amide rotamers: 1H NMR (300 MHz, DMSO-d6) δ 10.94 (br s, 1H), 10.38 (br s, 2H), 8.67-8.64 (m, 1H), 8.38-8.30 (m, 1H), 7.62-7.54 (m, 1H), 7.41-7.10 (m, 4H), 4.89-4.70 (m, 2H), 4.41-4.36 (m, 2H), 4.06-4.00 (m, 2H), 3.17-2.87 (m, 3H), 1.61-1.59 (m, 6H), 1.37-1.31 (m, 3H); MS (ESI) m/e 493 (M+H)+.