HRID1896437

反应详情

EQUATION

反应方程式

HRID 1896437 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

At room temperature, POCl3 (1 ml, 10.82 mmol, 2 eq) is added to a well stirred suspension of N,N-diethylaniline (1 ml, 5.41 mmol, 1 eq) and 1,3-dihydro-2H-indol-2-one x159 (0.72 g, 5.41 mmol, 1 eq) in dry toluene (15 ml). The mixture is heated at reflux during 3 hours. After cooling, water (15 ml) is carefully added and the organic layer is washed with water (3×25 ml). The organic layer is dried on anhydrous MgSO4, filtered off and concentrated under reduced pressure to obtain 0.76 g of 2-chloro-1H-indole x160 as an orange solid (0.76 g, 93%).

WORKUP

后处理

  1. temperatureThe mixture is heated
  2. temperatureat reflux during 3 hours
  3. temperatureAfter cooling
  4. washthe organic layer is washed with water (3×25 ml)
  5. dry with materialThe organic layer is dried on anhydrous MgSO4
  6. filtrationfiltered off
  7. concentrationconcentrated under reduced pressure