反应 #2006417

ord-c33bd6557c98445992fba955ff8c7bdf

反应方程式

COC(=O)c1ccc(C=O)cc1
4-carbomethoxybenzaldehyde
CC(=O)c1ccccc1
acetophenone
C[O-].[Na+]
sodium methoxide
Cl
HCl
COC(=O)c1ccc(C=CC(=O)c2ccccc2)cc1
Methyl-4-(3-oxo-3-phenylpropenyl)-benzoate

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度then heated
  2. 2
    温度to reflux for 1 hour
  3. 3
    温度cooled down to room temperature
  4. 4
    其他The layers were separated
  5. 5
    干燥the organic layer dried over anhydrous MgSO4
  6. 6
    过滤filtered
  7. 7
    其他The solvent was evaporated under vacuum
  8. 8
    其他to afford a yellow solid, which
  9. 9
    其他was recrystallized from acetonitrile/water
  10. 10
    其他to give a pale yellow crystalline solid

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: USRE043343E1uspto-grants-2012_05