HRID2286258

反应详情

EQUATION

反应方程式

HRID 2286258 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-5 °C

PROCEDURE

实验过程

A mixture of 144 g (1 mole) of 2-naphthol, 600 ml of diethyl ketone, 275 g (2 moles) of potassium carbonate and 850 g (4.5 moles) of 1,2-dibromoethane is refluxed for 48 hours. Diethyl ketone and excess dibromoethane are then distilled off under reduced pressure and the residue is taken up in 500 ml of methylene chloride and 200 ml of 10% strength sodium hydroxide solution. After the aqueous phase has been separated off, the organic layer is washed with 100 ml of water, dried over sodium sulfate and concentrated under reduced pressure. The solid residue is stirred with 100 ml of n-pentane for 10 minutes at -5° C., filtered and washed with 50 ml of cold pentane. There is obtained 195 g (78% of theory) of pure 1-bromo-2-(2-naphthyloxy)-ethane; m.p.: 93°-95° C.

WORKUP

后处理

  1. temperatureis refluxed for 48 hours
  2. distillationDiethyl ketone and excess dibromoethane are then distilled off under reduced pressure
  3. customAfter the aqueous phase has been separated off
  4. washthe organic layer is washed with 100 ml of water
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated under reduced pressure
  7. filtrationfiltered
  8. washwashed with 50 ml of cold pentane