反应详情

A solution of N-[2-(5-bromo-1-indolinyl)phenyl]phenyl-carbamate (11.5 g, 28.5 mmoles), N-methylpiperazine (15 ml) and ether (50 ml) was stirred at room temperature for 2 hours. The ether was evaporated. The mixture was filtered through a silica gel column (150 g), packed with dichloromethane, and the column was washed with 2% methanol-dichloromethane solution (2 1). The solvent was evaporated. The residue was purified by flash chromatography on a silica gel column (150 g, 230-400 mesh), eluted with 1% methanol/dichloromethane (4 1), 1.5% methanol/dichloromethane (2 1), and 2% methanol/dichloromethane. The fractions containing the desired material were collected and evaporated to give 10.9 g (90%) of product. Crystallization from chloroform and hexane afforded the analytical sample, mp 108°-110° C.

1. customThe ether was evaporated
2. filtrationThe mixture was filtered through a silica gel column (150 g)
3. washthe column was washed with 2% methanol-dichloromethane solution (2 1)
4. customThe solvent was evaporated
5. customThe residue was purified by flash chromatography on a silica gel column (150 g, 230-400 mesh)
6. washeluted with 1% methanol/dichloromethane (4 1), 1.5% methanol/dichloromethane (2 1), and 2% methanol/dichloromethane
7. additionThe fractions containing the desired material
8. customwere collected
9. customevaporated