HRID13944

反应详情

EQUATION

反应方程式

HRID 13944 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

To 6-chloro-4-methoxyindane (12.0 g, 0.072 mol) was added hydrogen bromide (30 wt. % in acetic acid, 325 mL) and the reaction mixture was stirred at 50° C. for 24 h. The reaction mixture was cooled to room temperature and diluted with ethyl acetate (750 mL), washed with water (3×500 mL), saturated aqueous sodium bicarbonate (2×500 m/L), saturated aqueous sodium chloride (500 mL), dried (sodium sulfate) and the solvent was removed in vacuo to provide a brown oil. Purification by flash column chromatography (silica, dichloromethane) provided 10.5 g (80%) of 6-chloroindan-4-ol as a pale yellow solid. mp 56-59° C.; Anal. calcd. for C9H9ClO.0.2H2O: C, 62.77; H, 5.50. Found: C, 62.75; H, 5.26.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. washwashed with water (3×500 mL), saturated aqueous sodium bicarbonate (2×500 m/L), saturated aqueous sodium chloride (500 mL)
  3. dry with materialdried (sodium sulfate)
  4. customthe solvent was removed in vacuo
  5. customto provide a brown oil
  6. customPurification by flash column chromatography (silica, dichloromethane)