反応 #50276

反応方程式

4-(2-bromotetrafluoroethoxy)benzaldehyde

water

→

4-Trifluoroethenyloxybenzaldehyde

収率 63.3%

溶媒

Acetonitrile

反応条件

後処理

1. 1
   workup.ADDITIONis added slowly
2. 2
   workup.ADDITIONaddition funnel
3. 3
   ろ過After filtration
4. 4
   その他to remove zinc salts and unreacted zinc
5. 5
   その他the acetonitrile is removed under vacuum on a rotary evaporator
6. 6
   workup.DISTILLATIONdistilled on a rotary evaporator under high vacuum (26.6 Pa)

実験手順

Acetonitrile (300 ml) and granular zinc (30.0 g) are combined in a 1 liter round bottomed flask and stirred at 75° C. under nitrogen as 4-(2-bromotetrafluoroethoxy)benzaldehyde (111.39 g, 0.37 mole) is added slowly by dropping addition funnel. The resulting mixture is stirred and heated at 79° C. for 12 hours. After filtration to remove zinc salts and unreacted zinc, the acetonitrile is removed under vacuum on a rotary evaporator. The resulting oily residue is flash distilled on a rotary evaporator under high vacuum (26.6 Pa) to provide 47.33 g (0.234 mole) of a water white oil in 63.3 percent yield.

出典