HRID590394

反应详情

EQUATION

反应方程式

HRID 590394 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of 3-(1H-indol-3-yl)propanoic acid (5 g, 0.026 mol) in DMF (20 mL) was added at 0° C. sodium hydride (2.11 g, 0.088 mol), the mixture was stirred some minutes at 0° C. and (2-bromoethoxy)(tert-butyl)dimethylsilane (5.67 mL, 0.026 mol) was added. The reaction mixture was stirred overnight at room temperature. The crude mixture was poured into a sodium sulphate saturate solution and extracted with ethyl acetate. The solvent was removed under reduced pressure and the crude obtained was purified over silica gel eluting with hexane:ether (100/0 to 0/100) to obtain the title compound (4g, 43%).

WORKUP

后处理

  1. stirringThe reaction mixture was stirred overnight at room temperature
  2. concentrationsaturate solution
  3. extractionextracted with ethyl acetate
  4. customThe solvent was removed under reduced pressure
  5. customthe crude obtained
  6. customwas purified over silica gel eluting with hexane