反应详情

tert-Butyl (1-{4-[2-(4-aminophenyl)-9H-imidazo[1,2-d]pyrido[2,3-b][1,4]benzodiazepin-3-yl]phenyl}cyclobutyl)carbamate (32.0 mg, 0.0561 mmol) was dissolved in DCM (1 mL). 4M HCl/dioxane (1 mL) was added to the mixture and stirred at room temperature for 6 hours. The mixture was concentrated and solidified with ether. The precipitated solids were collected by filtration and washed with ether to afford desired product (28.4 mg, 82.3%) as a pale red solid. 1HNMR (DMSO-d6) 400 MHz δ: 8.78 (br s, 3H), 8.66 (br s, 1H), 8.12 (dd, J=4.8, 1.6 Hz, 1H), 7.95 (dd, J=7.8, 1.4 Hz, 1H), 7.59-7.53 (m, 2H), 7.52-7.46 (m, 2H), 7.43-7.36 (m, 1H), 7.35-7.28 (m, 3H), 7.22-7.09 (m, 3H), 6.90 (dd, J=8.0, 1.6 Hz, 1H), 6.76 (dd, J=8.0, 4.8 Hz, 1H), 2.61-2.53 (m, 4H), 2.27-2.13 (m, 1H), 1.89-1.75 (m, 1H); LCMS: 471 [M+H].

1. concentrationThe mixture was concentrated
2. filtrationThe precipitated solids were collected by filtration
3. washwashed with ether