반응 #484787

반응 방정식

chlorotriphenylmethane methane

4-piperidone monohydrate hydrochloride

triethylamine

→

1-triphenylmethyl-4-piperidone

수율 103.5%

용매

dimethylformamide

반응 조건

후처리

1. 1
   workup.STIRRINGthe resulting mixture was stirring further for 5 hours at the same temperature
2. 2
   기타The triethylamine hydrochloride precipitated
3. 3
   온도by cooling
4. 4
   여과was filtered out
5. 5
   농축the filtrate was concentrated under reduced pressure
6. 6
   workup.ADDITIONTo the residue was added 150 ml of water
7. 7
   추출followed by extraction with 300 ml of ethyl acetate
8. 8
   세척The organic layer was then washed with saturated saline
9. 9
   건조dried over anhydrous magnesium sulfate
10. 10
    농축The solvent was concentrated under reduced pressure

실험 절차

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.

출처