반응 #595331

반응 방정식

4-hydroxybenzaldehyde

1-chloro-2-methyl-2-propanol

sodium carbonate

sodium bicarbonate

→

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

용매

DMF

ethyl acetate

반응 조건

후처리

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

실험 절차

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.

출처