反応 #2342

反応方程式

Sodium hydride

4-[4-(4-pyridyl)piperazin-1-yl]phenol

Allyl chloride

→

4-[4-(4-pyridyl)piperazin-1-yl]phenol allyl ether

収率 85.7%

溶媒

DMF

反応条件

後処理

1. 1
   workup.STIRRINGstirring
2. 2
   workup.WAITcontinued for 20 hours
3. 3
   抽出the mixture extracted three times with ethyl acetate
4. 4
   洗浄The combined extracts were washed with water and brine
5. 5
   乾燥dried (MgSO4)
6. 6
   その他evaporated
7. 7
   その他The residue was triturated with hexane
8. 8
   ろ過filtered

実験手順

Sodium hydride (60% dispersion in mineral oil, 0.4 g) was added to a stirred suspension of 4-[4-(4-pyridyl)piperazin-1-yl]phenol (2.55 g) in DMF (25 ml) and the mixture stirred for 20 minutes at room temperature. Allyl chloride (0.756 g) was added dropwise and stirring continued for 20 hours. Ice-water (75 ml) was added and the mixture extracted three times with ethyl acetate. The combined extracts were washed with water and brine, dried (MgSO4) and evaporated. The residue was triturated with hexane and filtered to give 4-[4-(4-pyridyl)piperazin-1-yl]phenol allyl ether (2.5 g) as a solid;

出典