Reaktion #484787

Reaktionsgleichung

chlorotriphenylmethane methane

4-piperidone monohydrate hydrochloride

triethylamine

→

1-triphenylmethyl-4-piperidone

Ausbeute 103.5%

Lösungsmittel

dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGthe resulting mixture was stirring further for 5 hours at the same temperature
2. 2
   SonstigeThe triethylamine hydrochloride precipitated
3. 3
   Temperaturby cooling
4. 4
   Filtrationwas filtered out
5. 5
   Einengenthe filtrate was concentrated under reduced pressure
6. 6
   workup.ADDITIONTo the residue was added 150 ml of water
7. 7
   Extraktionfollowed by extraction with 300 ml of ethyl acetate
8. 8
   WaschenThe organic layer was then washed with saturated saline
9. 9
   Trocknendried over anhydrous magnesium sulfate
10. 10
    EinengenThe solvent was concentrated under reduced pressure

Vorschrift

After the portionwise addition of 18.1 g (65.1 mmol) of chlorotriphenylmethane methane to a 150 ml dimethylformamide solution of 10.0 g (65.1 mmol) of 4-piperidone monohydrate hydrochloride and 20.0 g (198 mmol) of triethylamine at 60° C. under stirring, the resulting mixture was stirring further for 5 hours at the same temperature. The triethylamine hydrochloride precipitated by cooling was filtered out and the filtrate was concentrated under reduced pressure. To the residue was added 150 ml of water, followed by extraction with 300 ml of ethyl acetate. The organic layer was then washed with saturated saline and dried over anhydrous magnesium sulfate. The solvent was concentrated under reduced pressure, whereby 23.0 g (yield: 98.3%) of 1-triphenylmethyl-4-piperidone were obtained.

Quelle