反応 #2553

反応方程式

4-(4-fluorobenzoyl)piperidine

2-bromoethanol

→

title compound

収率 78.0%

4-(4-Fluorobenzoyl)-1-(2-hydroxyethyl)piperidine

収率 78.0%

溶媒

triethylamine

反応条件

後処理

1. 1
   温度After 1 hour of heating
2. 2
   温度under reflux
3. 3
   その他triethylamine was removed by evaporation
4. 4
   workup.ADDITIONthe resulting residue was mixed with saturated sodium carbonate aqueous solution (40 ml)
5. 5
   抽出extracted with ethyl acetate
6. 6
   乾燥The resulting organic layer was dried on anhydrous sodium carbonate
7. 7
   その他the solvent was removed by evaporation
8. 8
   その他the resulting residue was purified

実験手順

In an atmosphere of argon, 4-(4-fluorobenzoyl)piperidine (2.07 g, 10 mmol) was dissolved in triethylamine (30 ml) to which was subsequently added dropwise 2-bromoethanol (1.1 ml, 14.7 mmol) at room temperature. After 1 hour of heating under reflux, triethylamine was removed by evaporation, and the resulting residue was mixed with saturated sodium carbonate aqueous solution (40 ml) and extracted with ethyl acetate. The resulting organic layer was dried on anhydrous sodium carbonate, the solvent was removed by evaporation and then the resulting residue was purified by subjecting it to a silica gel column chromatography (ethyl acetate-methylene chloride:methanol=10:1) to obtain 1.96 g (78.0%) of the title compound in the form of light yellow solid.

出典