反应详情

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.

1. stirringthe resulting mixture was stirring further for 5 hours at the same temperature
2. customThe triethylamine hydrochloride precipitated
3. temperatureby cooling
4. filtrationwas filtered out
5. concentrationthe filtrate was concentrated under reduced pressure
6. additionTo the residue was added 150 ml of water
7. extractionfollowed by extraction with 300 ml of ethyl acetate
8. washThe organic layer was then washed with saturated saline
9. dry with materialdried over anhydrous magnesium sulfate
10. concentrationThe solvent was concentrated under reduced pressure