HRID1978626

反应详情

EQUATION

反应方程式

HRID 1978626 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

To a solution of 4-bromo-N-ethylaniline (17.08 g) in DMF (100 ml) were added at room temperature potassium carbonate (17.1 g), sodium iodide (12.4 g) and 2-bromoethylethyl ether (10.2 ml), and the mixture was stirred at 90° C. for 24 hours. To the mixture were added 2-bromoethylethyl ether (5.0 ml), potassium carbonate (6.22 g) and sodium iodide (6.64 g), and the mixture was stirred for 2 days. To the mixture were added 2-bromoethylethyl ether (10.0 ml), potassium carbonate (17.1 g) and sodium iodide (12.4 g), and the mixture was stirred at 90° C. for 3 days. To the mixture was added water, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine and dried with magnesium sulfate. Under reduced pressure, the solvent was evaporated, and the residue was purified with silica gel column chromatography (ethyl acetate/hexane=1:9) to give yellow oil of 4-bromo-N-(2-propoxyethyl)-N-ethylaniline (18.11 g).

WORKUP

后处理

  1. stirringthe mixture was stirred for 2 days
  2. stirringthe mixture was stirred at 90° C. for 3 days
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with saturated brine
  5. dry with materialdried with magnesium sulfate
  6. customUnder reduced pressure, the solvent was evaporated
  7. customthe residue was purified with silica gel column chromatography (ethyl acetate/hexane=1:9)