反应详情

A mixture of phenyl N-(5-phenyl-2-pyrazinyl)carbamate 1-2 (7,350 mg, 1.20 mmol), 1-methylsulfonylspiro[indoline-3,4′-piperidine]hydrochloride 1-3 (400 mg, 1.32 mmol) and Et3N (0.5 mL, 3.6 mmol) in CHCl3 (6 mL) was heated to reflux for 3 h. After cooling, the mixture was diluted with EtOAc, washed with 10% citric acid, sat. NaHCO3 and brine, dried over MgSO4, and concentrated under reduced pressure to start precipitation. The precipitate was collected by filtration and dried in vacuo to give 100 (517 mg, 93%) as a white powder.

1. temperaturewas heated
2. temperatureto reflux for 3 h
3. temperatureAfter cooling
4. washwashed with 10% citric acid, sat. NaHCO3 and brine
5. dry with materialdried over MgSO4
6. concentrationconcentrated under reduced pressure
7. customprecipitation
8. filtrationThe precipitate was collected by filtration
9. customdried in vacuo