反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
tert-Butyl (1-{4-[2-(4-acetamidophenyl)-9H-imidazo[1,2-d]pyrido[2,3-b][1,4]benzodiazepin-3-yl]phenyl}cyclobutyl)carbamate (22.6 mg, 0.0369 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 (21.5 mg, 93.5%) as pale yellow solid. 1HNMR (DMSO-d6) 400 MHz δ: 10.08 (s, 1H), 8.70 (br s, 2H), 8.64 (s, 1H), 8.11 (dd, J=4.8, 1.6 Hz, 1H), 7.95 (dd, J=7.8, 1.8 Hz, 1H), 7.58-7.49 (m, 4H), 7.44-7.36 (m, 3H), 7.34-7.28 (m, 3H), 7.17-7.10 (m, 1H), 6.89 (dd, J=8.0, 1.6 Hz, 1H), 6.75 (dd, J=7.8, 4.6 Hz, 1H), 2.65-2.39 (m, 4H), 2.26-2.13 (m, 1H), 2.04 (s, 3H), 1.89-1.75 (m, 1H); LCMS: 513 [M+H].
WORKUP
后处理
- concentrationThe mixture was concentrated
- filtrationThe precipitated solids were collected by filtration
- washwashed with ether