HRID1358003
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
- 120 °C
PROCEDURE
实验过程
A solution of 6-methoxy-1-[4-(phenylmethoxy)benzyl]-1,2,3,4-tetrahydroisoquinoline (2.10 g, 5.84 mmol) and 1-fluoro-4-nitrobenzene (1.65 g, 11.7 mmol) in 40 mL of DMSO was treated with powdered K2CO3 (1.62 g, 11.7 mmol) and the reaction mixture was warmed at 120° C. for 12 h. The reaction mixture was cooled to room temperature and 300 mL of water was added. The aqueous layer was extracted with CH2Cl2 and the combined organic layer was washed with water, dried over MgSO4, then concentrated under reduced pressure. The crude product was purified by flash chromatography to provide the title compound (2.50 g, 89%). ES-MS, (m/z) 481 [M+H]+.
WORKUP
后处理
- temperatureThe reaction mixture was cooled to room temperature
- extractionThe aqueous layer was extracted with CH2Cl2
- washthe combined organic layer was washed with water
- dry with materialdried over MgSO4
- concentrationconcentrated under reduced pressure
- customThe crude product was purified by flash chromatography