반응 #2554

반응 방정식

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

DMF

thionyl chloride

→

title compound

수율 96.3%

1-(2-Chloroethyl)-4-(4-fluorobenzoyl)piperidine hydrochloride

수율 96.3%

용매

methylene chloride

반응 조건

후처리

1. 1
   온도with cooling in an ice bath
2. 2
   기타the solvent was removed by evaporation
3. 3
   workup.DISTILLATIONthe resulting residue was subjected to azeotropic distillation
4. 4
   세척Thereafter, the thus obtained residue was washed with an ether-methylene chloride (4:1) mixture solution (30 ml)

실험 절차

In an atmosphere of dry air, 4-(4-fluorobenzoyl)-1-(2-hydroxyethyl)piperidine (1.96 g, 7.8 mmol) was dissolved in methylene chloride (10 ml) to which, with cooling in an ice bath, were subsequently added dropwise DMF (0.1 ml) and thionyl chloride (2.5 ml, 34.2 mmol). After 7 hours of stirring at room temperature, the solvent was removed by evaporation, and the resulting residue was subjected to azeotropic distillation using benzene (15 ml×2). Thereafter, the thus obtained residue was washed with an ether-methylene chloride (4:1) mixture solution (30 ml) to obtain 2.3 g (96.3%) of the title compound in the form of light beige powder.

출처