反応 #595331

反応方程式

4-hydroxybenzaldehyde

1-chloro-2-methyl-2-propanol

sodium carbonate

sodium bicarbonate

→

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

溶媒

DMF

ethyl acetate

反応条件

後処理

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

実験手順

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.

出典