反应 #595331

反应方程式

4-hydroxybenzaldehyde

1-chloro-2-methyl-2-propanol

sodium carbonate

sodium bicarbonate

→

4-(2-Hydroxy-2-methylpropoxy)benzaldehyde

溶剂

DMF

ethyl acetate

反应条件

后处理

1. 1
   温度under reflux for 24 h
2. 2
   其他The phases are separated
3. 3
   干燥the organic phase is dried over magnesium sulfate
4. 4
   其他After removal of the solvent
5. 5
   其他the residue is purified by column chromatography on silica gel 60 (mobile phase gradient: cyclohexane/ethyl acetate 5:1→1:1)
6. 6
   其他This gives a reddish solid which
7. 7
   其他is used without further purification for the subsequent step

实验过程

5.00 g (40.94 mmol) of 4-hydroxybenzaldehyde, 4.44 g (40.94 mmol) of 1-chloro-2-methyl-2-propanol and 6.08 g (57.32 mmol) of sodium carbonate are initially charged in 50 ml of dry DMF and stirred under reflux for 24 h. After cooling to RT, 20 ml of ethyl acetate and 20 ml of sat. aqueous sodium bicarbonate solution are added. The phases are separated, and the organic phase is dried over magnesium sulfate. After removal of the solvent, the residue is purified by column chromatography on silica gel 60 (mobile phase gradient: cyclohexane/ethyl acetate 5:1→1:1). This gives a reddish solid which is used without further purification for the subsequent step.

来源