Reaktion #735834

Reaktionsgleichung

sulfuric acid

α-(3-methyl-phenyl)-2-piperidino-benzyl alcohol

ethyl 4-cyanomethyl-benzoate

→

Ethyl 4-{N-[α-[3-methyl-phenyl)-2-piperidino-benzyl]-aminocarbonylmethyl}-benzoate

Lösungsmittel

o-dichlorobenzene

o-dichlorobenzene

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONthe mixture was poured onto ice water
2. 2
   Extraktionextracted once with ether
3. 3
   Extraktionextracted with chloroform
4. 4
   ExtraktionThe chloroform extract
5. 5
   Einengenwas concentrated by evaporation
6. 6
   Sonstigethe residue was recrystallized from ethanol

Vorschrift

A mixture of 0.22 gm (0.8 m mol) of α-(3-methyl-phenyl)-2-piperidino-benzyl alcohol and 0.15 gm (0.8 m mol) of ethyl 4-cyanomethyl-benzoate in 2 ml of o-dichlorobenzene was added dropwise, at ambient temperature, to 1.5 ml of o-dichlorobenzene and 1.5 ml of concentrated sulfuric acid. After stirring for two hours, the mixture was poured onto ice water, extracted once with ether, made alkaline with dilute sodium hydroxide solution, and extracted with chloroform. The chloroform extract was concentrated by evaporation, and the residue was recrystallized from ethanol.

Quelle