反应 #94744

反应方程式

1-(3',4'-dimethoxyphenyl)-7-phenyl-2-nitro-5-heptanone

p-toluenesulfonic acid

ethylene glycol

→

oil

1-(3',4'-dimethoxyphenyl)-7-phenyl-2-nitro-5-heptanone ethylene ketal

溶剂

cyclohexane

反应条件

后处理

1. 1
   其他flask equipped with a Dean Stark trap
2. 2
   温度to reflux overnight
3. 3
   浓缩concentrated in vacuo
4. 4
   workup.ADDITIONDil NaHCO3 solution was added to the residue
5. 5
   萃取extracted with ethyl acetate
6. 6
   干燥dried over anh. MgSO4
7. 7
   过滤filtered
8. 8
   浓缩concentrated under reduced pressure

实验过程

Into a 1 l r.b. flask equipped with a Dean Stark trap was placed 46.4 g (0.12 m) of 1-(3',4'-dimethoxyphenyl)-7-phenyl-2-nitro-5-heptanone, 1.5 g p-toluenesulfonic acid, 50 mL of ethylene glycol and 300 mL of cyclohexane. The mixture was allowed to reflux overnight, then concentrated in vacuo. Dil NaHCO3 solution was added to the residue and extracted with ethyl acetate. The organic layer was backwashed with water, dried over anh. MgSO4, filtered and concentrated under reduced pressure to give 45.3 g of an oil which solidified on drying at room temperature under vacuum.

来源