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
- 85 °C
PROCEDURE
实验过程
To a mixture of 7-(2-chloroethoxy)-1-phenyl-1,2-dihydro[1,4]oxazino[2,3,4-jk]carbazole (0.453 g, 1.24 mmol) in dry DMF (6 mL) is added tert-butyl-1-piperazinecarboxylate (0.232 g, 1.24 mmol), sodium iodide (0.018 g, 0.124 mmol), and potassium carbonate (0.342 g, 2.48 mmol). The mixture is heated at 85° C. for 20 h. The mixture is then cooled and partitioned between Et2O and water. The organic layer is washed twice with water (200 mL), dried over anhydrous sodium sulfate and concentrated. Column chromatography (50 mL silica) using CH2Cl2/CH3OH (98/2) yielded 0.487 g (76%) of tert-butyl 4-{2-[(1-phenyl-1,2-dihydro[1,4]oxazino[2,3,4-jk]carbazol-7-yl)oxy]ethyl}-1-piperazinecarboxylate; mp 72° C.;.
WORKUP
后处理
- temperatureThe mixture is then cooled
- custompartitioned between Et2O and water
- washThe organic layer is washed twice with water (200 mL)
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated