反应详情

温度

60 °C

5-chloro-1-(4-fluorophenyl)indole (6.70 kg) and 4-piperidone-mono-hydrate,hydrochloride (8.38 kg) were transferred to a 200 L reactor under N2 cover. Acetic acid (67 L) was added and the reaction mixture was heated to 60° C. Concentrated HCl (37%, 33.5 L) was added during ½ hour and then the mixture was heated to the reflux temperature (85° C.) and refluxed for 1 hour (final temperature 95° C.). After cooling to 30° C., 33.5 L acetone was added followed by further cooling to 25° C. Filtration, wash (acetone 20 L) and drying in vacuum at 60° C. gave the title product as a white powder, yield 8.94 kg.

1. temperaturethe mixture was heated to the reflux temperature (85° C.)
2. temperaturerefluxed for 1 hour (final temperature 95° C.)
3. temperatureAfter cooling to 30° C.
4. temperatureby further cooling to 25° C
5. filtrationFiltration
6. washwash (acetone 20 L)
7. customdrying in vacuum at 60° C.