反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of tert-butyl (1-{4-[2-(1,3-thiazol-2-yl)-9H-imidazo[1,2-d]pyrido[2,3-b][1,4]benzodiazepin-3-yl]phenyl}cyclobutyl)carbamate (302 mg, 0.54 mmol) and 4N HCl/dioxane (1.5 ml) in dichloromethane (10 ml) was stirred at room temperature for 16 hours and diluted with diethyl ether. The precipitate was collected on a filter paper and dried to give a yellow solid (76%). 1HNMR (DMSO-d6) 400 MHz δ: 8.79 (m, 2H), 8.69 (s, 1H), 8.13 (dd, J=4.9, 1.4 Hz, 1H), 7.93 (dd, J=7.7, 1.4 Hz, 1H), 7.76 (d, J=2.9 Hz, 1H), 7.72 (d, J=2.9 Hz, 1H), 7.56-7.50 (m, 4H), 7.40 (td, J=7.7, 1.7 Hz, 1H), 7.33 (d, J=7.5 Hz, 1H), 7.15 (td, J=7.5, 1.2 Hz, 1H) 6.91 (dd, J=8.0, 1.7 Hz, 1H), 6.76 (dd, J=8.0, 4.6 Hz, 1H), 2.60-2.55 (m, 4H), 2.25-2.15 (m, 1H), 1.86-1.76 (m, 1H); LC/MS [M+H]: 463.
WORKUP
后处理
- customThe precipitate was collected on a filter paper
- customdried