反応 #2554

反応方程式

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

DMF

thionyl chloride

→

title compound

収率 96.3%

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

収率 96.3%

溶媒

methylene chloride

反応条件

後処理

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

実験手順

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.

出典