HRID585455

反应详情

EQUATION

反应方程式

HRID 585455 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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 (0.273 g, 0.751 mmol) in dry DMF (10 mL) is added sodium iodide (0.113 g, 0.751 mmol), potassium carbonate (0.207 g, 1.5 mmol), and ethanolamine (0.046 g, 0.751 mmol). The mixture is heated at 85° C. for 17 h. The temperature is then increased to 90° C. and the mixture is allowed to stir for another 5 h. The mixture is then cooled to room temperature and partitioned between water and ether. The organic layer is washed twice with water (50 mL), dried over anhydrous sodium sulfate and concentrated. Column chromatography (50 mL silica gel) using 5% methanol in CH2Cl2 gave 0.123 g (42%) of 2-({2-[(1-phenyl-1,2-dihydro[1,4]oxazino[2,3,4-jk]carbazol-7-yl)oxy]ethyl}amino)-1-ethanol.

WORKUP

后处理

  1. temperatureThe temperature is then increased to 90° C.
  2. temperatureThe mixture is then cooled to room temperature
  3. custompartitioned between water and ether
  4. washThe organic layer is washed twice with water (50 mL)
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated