Reaktion #2320115

Reaktionsgleichung

α-chloroethyl chloroformate

1-Benzyl-4-(4-chloro-3-trifluoromethyl-phenyl)-piperidine

→

title compound

4-(4-chloro-3-trifluoromethyl-phenyl)-piperidine

HCl

Lösungsmittel

1,2-dichloroethane

1,2-dichloroethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwas added dropwise at 0° C
2. 2
   Temperaturto reflux for 2 days
3. 3
   SonstigeThe volatiles were evaporated in vacuo
4. 4
   Sonstigethe residue triturated with methanol
5. 5
   Temperaturto reflux for 4 hours
6. 6
   SonstigeThe solvent was evaporated

Vorschrift

A solution of 1-Benzyl-4-(4-chloro-3-trifluoromethyl-phenyl)-piperidine (1.1 g) in 1,2-dichloroethane (50 ml) was cooled to 0° C. Then α-chloroethyl chloroformate (1.5 g) dissolved in 1,2-dichloroethane (30 ml) was added dropwise at 0° C. The reaction mixture was then brought to reflux for 2 days. The volatiles were evaporated in vacuo and the residue triturated with methanol. The mixture was brought to reflux for 4 hours. The solvent was evaporated to afford the title compound as HCl salt (light brown crystals, 1.0 g) MS m/z (relative intensity, 70 eV) 263 (M+, 34), 262 (22), 83 (22), 57 (60), 56 (bp).

Quelle