HRID1438865

反应详情

EQUATION

反应方程式

HRID 1438865 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

While stirring and under nitrogen, a mixture of 3.14 g (0.15 mol) of 2-(4'-hydroxy-phenyl)-indole, prepared as in Example 2, 2.1 g of anhydrous potassium carbonate and 100 ml of anhydrous acetone was refluxed and a solution of 50 ml of anhydrous acetone containing 1.8 ml (0.015 mol) of benzyl bromide was then added, drop-by-drop. The solution was heated for 4 hours and 0.4 ml (0.003 mole) of benzyl bromide was added with 0.5 g of potassium carbonate. Heating was continued for 4 hours and the hot solution was filtered. The filter was washed with 50 ml of acetone, the filtrate was concentrated under vacuum and was taken up in 100 ml of boiling methylethylketone. The hot reaction medium was filtered and the filtrate was cooled in an ice-bath for 30 minutes. The precipitate which was obtained was centrifuged and recrystallized from methylethylketone to give 3.3 g of 2-(4'-benzyloxy-phenyl)-indole.

WORKUP

后处理

  1. temperaturewas refluxed
  2. temperatureThe solution was heated for 4 hours
  3. temperatureHeating
  4. filtrationthe hot solution was filtered
  5. washThe filter was washed with 50 ml of acetone
  6. concentrationthe filtrate was concentrated under vacuum
  7. filtrationThe hot reaction medium was filtered
  8. temperaturethe filtrate was cooled in an ice-bath for 30 minutes
  9. customThe precipitate which was obtained
  10. customrecrystallized from methylethylketone