반응 #2006417

반응 방정식

4-carbomethoxybenzaldehyde

acetophenone

sodium methoxide

HCl

→

Methyl-4-(3-oxo-3-phenylpropenyl)-benzoate

용매

methanol

EtOAc

반응 조건

후처리

1. 1
   온도then heated
2. 2
   온도to reflux for 1 hour
3. 3
   온도cooled down to room temperature
4. 4
   기타The layers were separated
5. 5
   건조the organic layer dried over anhydrous MgSO4
6. 6
   여과filtered
7. 7
   기타The solvent was evaporated under vacuum
8. 8
   기타to afford a yellow solid, which
9. 9
   기타was recrystallized from acetonitrile/water
10. 10
    기타to give a pale yellow crystalline solid

실험 절차

To 4-carbomethoxybenzaldehyde (79 mg, 0.48 mmol) and acetophenone (56 μL, 0.48 mmol) in anhydrous methanol (1.6 mL), was added neat sodium methoxide (26 mg, 0.48 mmol). The mixture was stirred at room temperature overnight then heated to reflux for 1 hour, cooled down to room temperature and added HCl 1N and EtOAc. The layers were separated and the organic layer dried over anhydrous MgSO4 and filtered. The solvent was evaporated under vacuum to afford a yellow solid, which was recrystallized from acetonitrile/water to give a pale yellow crystalline solid.

출처