تفاعل #2554

معادلة التفاعل

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

DMF

thionyl chloride

→

title compound

المردود 96.3%

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

المردود 96.3%

المذيبات

methylene chloride

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.

المصدر