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
To a solution of tert-butyl {1-methyl-1-[4-(2-phenyl-9H-imidazo[1,2-d]pyrido[2,3-b][1,4]benzodiazepin-3-yl)phenyl]ethyl}carbamate (41 mg) in dichloromethane (4 mL) was added hydrogen chloride in 1,4-dioxane (2.5 mL) dropwise at room temperature. After being stirred at the same temperature for 5 h, the reaction mixture was concentrated under reduced pressure. The residue was suspended with ethyl acetate and filtered to give the product (37 mg, 85%). 1HNMR (DMSO-d6) 400 MHz δ: 8.72-8.62 (m, 3H), 8.11 (dd, J=4.6, 1.8 Hz, 1H), 7.96 (dd, J=7.8, 1.4 Hz, 1H), 7.57 (d, J=8.7 Hz, 2H), 7.52-7.47 (m, 2H), 7.42-7.25 (m, 7H), 7.17-7.11 (m, 1H), 6.88 (dd, J=8.0, 1.8 Hz, 1H), 6.74 (dd, J=8.0, 4.6 Hz, 1H), 1.63 (s, 6H). LCMS: 444 [M+H].
WORKUP
后处理
- concentrationthe reaction mixture was concentrated under reduced pressure
- filtrationfiltered