反应详情

温度

70 °C

A suspension of 2-(6-Bromo-pyridin-2-ylmethyl)-isoindole-1,3-dione (4000 mg, 12.61 mmol) in ethanol (60 mL ) was heated at 70° C. until complete dissolution was observed. Hydrazine hydrate (3156 mg, 63.06 mmol) was then added and the resulting mixture was heated at 70° C. for 5 h. The resulting solution was cooled to 0° C. and filtered. The filtrate was concentrated in vacuo and the crude residue was purified by column chromatography with a gradient of 0 to 30% methanol/dichloromethane to give C-(6-Bromo-pyridin-2-yl)-methylamine as a yellow solid (2070 mg, 79%). MS ES (MH+187.1, RT=1.11 min).

1. temperaturethe resulting mixture was heated at 70° C. for 5 h
2. temperatureThe resulting solution was cooled to 0° C.
3. filtrationfiltered
4. concentrationThe filtrate was concentrated in vacuo
5. customthe crude residue was purified by column chromatography with a gradient of 0 to 30% methanol/dichloromethane