HRID1585967

反应详情

EQUATION

反应方程式

HRID 1585967 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To the crude product of benzindanol dissolved in 200 ml of toluene was added 1.2 g (6.3 mmole) of p-toluenesulfonic acid, and the mixture was stirred at 80° C. for 15 minutes. The reaction was terminated with a saturated aqueous sodium hydrogen carbonate solution. The mixture was extracted with toluene, and the organic phase was washed with a saturated aqueous sodium hydrogen carbonate solution and a saturated aqueous sodium chloride solution, dried over magnesium sulfate, and concentrated under reduced pressure. The crude product of benzindene was obtained in an amount of 12.6 g, which was purified by column chromatography (Merck; solvent, hexane-ethyl acetate 0-1%). The product was obtained in an amount of 9.66 g (yield 85%).

WORKUP

后处理

  1. customThe reaction was terminated with a saturated aqueous sodium hydrogen carbonate solution
  2. extractionThe mixture was extracted with toluene
  3. washthe organic phase was washed with a saturated aqueous sodium hydrogen carbonate solution
  4. dry with materiala saturated aqueous sodium chloride solution, dried over magnesium sulfate
  5. concentrationconcentrated under reduced pressure