HRID1174436

反应详情

EQUATION

反应方程式

HRID 1174436 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

In a four-aperture flask, 9.6 g (70 mmol) of p-aminophenethyl alcohol, 38.7 g (280 mmol) of potassium carbonate, and 100 mL of monochlorobenzene were poured, and the mixture was heated at 120° C. under an argon atmosphere with stirring. Then, 32.8 g (210 mmol) of ethyl iodide was delivered by drops into the mixture for 5 hours. Upon completion of the dripping, the mixture was further heated with stirring for 5 hours. The reaction solution was cooled to the room temperature and then diluted with dichloromethane, followed by washing with water three times. The dichloromethane solution was dried with anhydrous magnesium sulfate, the solvent was distilled away to purify the dichloromethane solution by silica gel chromatography using a mixture solvent of toluene/ethyl acetate (2/1) as an eluent to thereby synthesize 12.1 g (yield: 89% by mass) of p-diethylaminophenethyl alcohol.

WORKUP

后处理

  1. temperatureUpon completion of the dripping, the mixture was further heated
  2. stirringwith stirring for 5 hours
  3. temperatureThe reaction solution was cooled to the room temperature
  4. washby washing with water three times
  5. dry with materialThe dichloromethane solution was dried with anhydrous magnesium sulfate
  6. distillationthe solvent was distilled away
  7. customto purify the dichloromethane solution by silica gel chromatography
  8. customto thereby synthesize 12.1 g (yield: 89% by mass) of p-diethylaminophenethyl alcohol