HRID241088
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
CONDITIONS
反应条件
- 温度
- 160 °C
PROCEDURE
实验过程
A mixture of 7-bromo-2,3,4,5-tetrahydro-1,4-benzoxazepine hydrochloride (300 mg, 1.13 mmol), 4-chloro-6,7-dimethoxyquinoline (253 mg, 1.13 mmol), and potassium carbonate (470 mg, 3.40 mmol) in N-methylpyrrolidine (2 mL) was stirred at 160° C. for 17 h. Ethyl acetate (75 mL) was added and the mixture was washed with water (3×25 mL) and brine (25 mL), dried over sodium sulfate, and concentrated. Column chromatography on silica (dichloromethane:methanol 95:5) afforded 4-[6,7-bis(methyloxy)quinolin-4-yl]-7-bromo-2,3,4,5-tetrahydro-1,4-benzoxazepine (80 mg). MS (EI) for C20H19BrN2O3: 416 (MH+).
WORKUP
后处理
- washthe mixture was washed with water (3×25 mL) and brine (25 mL)
- dry with materialdried over sodium sulfate
- concentrationconcentrated