تفاعل #595331

معادلة التفاعل

4-hydroxybenzaldehyde

1-chloro-2-methyl-2-propanol

sodium carbonate

sodium bicarbonate

→

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

المذيبات

DMF

ethyl acetate

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةunder reflux for 24 h
2. 2
   أخرىThe phases are separated
3. 3
   تجفيفthe organic phase is dried over magnesium sulfate
4. 4
   أخرىAfter removal of the solvent
5. 5
   أخرىthe residue is purified by column chromatography on silica gel 60 (mobile phase gradient: cyclohexane/ethyl acetate 5:1→1:1)
6. 6
   أخرىThis gives a reddish solid which
7. 7
   أخرىis used without further purification for the subsequent step

الإجراء التجريبي

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.

المصدر