HRID1587802
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
- 4 °C
PROCEDURE
实验过程
Anhydrous potassium carbonate (2.76 g) was added to a stirred solution of 4-chloro-2-cyanophenol (1.53 g) and 2-bromo-2-methyl propanal (2.26 g) in THF (50 ml) and the mixture heated at reflux for 5 hours. The mixture was then cooled to 4° C., the suspended solid removed by filtration and the filtrate evaporated to give a yellow oil which crystallised on standing. The solid was triturated with hexane and collected by filtration to give 2-(4-chloro-2-cyanophenoxy)-2-methylpropanal (2.11 g), m.p. 85°-88° C.; NMR: 1.52(6H,s), 6.79(1H,d,J=8 Hz), 7.42(1H,dd,J=8,2.5 Hz), 7.57(1H,d,J=2.5 Hz), 9.80(1H,s).
WORKUP
后处理
- temperaturethe mixture heated
- temperatureat reflux for 5 hours
- customthe suspended solid removed by filtration
- customthe filtrate evaporated
- customto give a yellow oil which
- customcrystallised
- customThe solid was triturated with hexane
- filtrationcollected by filtration