反应详情

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-propoxy-3-trifluoromethoxybenzyl)acrylamide (0.255 g, 0.503 mmol) in CH2Cl2 (5 mL) under N2, was treated with anhydrous HCl (0.25 mL of a 2 M solution in diethyl ether, 0.5 mmol). After stirring for 18 h, the resulting solid was collected by filtration and washed with Et2O (150 mL). The solid was dried under vacuum to yield the target compound (0.21 g, 82%) as an off white solid and as a mixture of amide rotamers: 1H NMR (300 MHz, DMSO-d6) δ 10.93-10.91 (m, 1H), 10.51 (br s, 2H), 8.66-8.64 (m, 1H), 8.40-8.32 (m, 1H), 7.63-7.54 (m, 1H), 7.40-7.09 (m, 4H), 4.89-4.70 (m, 2H), 4.41-4.36 (m, 2H), 3.96-3.90 (m, 2H), 3.18-2.87 (m, 3H), 1.79-1.70 (m, 2H), 1.63-1.61 (m, 6H), 1.09-0.97 (m, 3H); MS (ESI) m/e 507 (M+H)+.

1. filtrationthe resulting solid was collected by filtration
2. washwashed with Et2O (150 mL)
3. customThe solid was dried under vacuum