反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureis refluxed for 48 hours
- distillationDiethyl ketone and excess dibromoethane are then distilled off under reduced pressure
- customAfter the aqueous phase has been separated off
- washthe organic layer is washed with 100 ml of water
- dry with materialdried over sodium sulfate
- concentrationconcentrated under reduced pressure
- filtrationfiltered
- washwashed with 50 ml of cold pentane