反应详情

To a stirred suspension of lithium aluminum hydride (400 mg) in THF (25 ml) was added a solution of ethyl(2-amino-5-bromo-3-methylphenyl)carbamate (1 g) in THF (10 ml) at 0° C. The mixture was then warmed to room temperature, followed by heating at reflux for 1 h. The reaction mixture was cooled to 0° C., diluted with THF (45 ml) and a saturated Na2SO4 solution was added dropwise thereto. The mixture was further stirred for 30 min and solids were filtered over Celite. The filtrate was concentrated in vacuo. The residue was purified by silica gel column chromatography (hexane/EtOAc) to give the title compound (550 mg) as a brownish liquid.

1. temperatureby heating
2. temperatureat reflux for 1 h
3. temperatureThe reaction mixture was cooled to 0° C.
4. filtrationsolids were filtered over Celite
5. concentrationThe filtrate was concentrated in vacuo
6. customThe residue was purified by silica gel column chromatography (hexane/EtOAc)