反応 #94744

反応方程式

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

溶媒

cyclohexane

反応条件

後処理

1. 1
   その他flask equipped with a Dean Stark trap
2. 2
   温度to reflux overnight
3. 3
   濃縮concentrated in vacuo
4. 4
   workup.ADDITIONDil NaHCO3 solution was added to the residue
5. 5
   抽出extracted with ethyl acetate
6. 6
   乾燥dried over anh. MgSO4
7. 7
   ろ過filtered
8. 8
   濃縮concentrated under reduced pressure

実験手順

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.

出典