반응 #2553

반응 방정식

4-(4-fluorobenzoyl)piperidine

2-bromoethanol

→

title compound

수율 78.0%

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

수율 78.0%

용매

triethylamine

반응 조건

후처리

1. 1
   온도After 1 hour of heating
2. 2
   온도under reflux
3. 3
   기타triethylamine was removed by evaporation
4. 4
   workup.ADDITIONthe resulting residue was mixed with saturated sodium carbonate aqueous solution (40 ml)
5. 5
   추출extracted with ethyl acetate
6. 6
   건조The resulting organic layer was dried on anhydrous sodium carbonate
7. 7
   기타the solvent was removed by evaporation
8. 8
   기타the resulting residue was purified

실험 절차

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.

출처