反应详情

温度

80 °C

4-(5-Bromo-6-nitropyridin-3-yl)morpholine (95 mg, 0.33 mmol) was dissolved in EtOH (12 mL) and water (3.0 mL) was added, followed by SnCl2 (313 mg, 1.65 mmol). The reaction mixture was heated to 80° C. for 2 h, cooled to room temperature and diluted with DCM. The two phases were separated, the organic phase was washed with water. The water phase was back extracted with DCM. The pH was adjusted to 12 with 6N NaOH and the mixture was further extracted with DCM. The organic extracts were combined, dried (Na2SO4) and evaporated under reduced pressure obtaining the desired 3-bromo-5-morpholinopyridin-2-amine (71.5 mg, 84%). LCMS (m/z): 260.0 (MH+), 0.37 min.

1. temperaturecooled to room temperature
2. customThe two phases were separated
3. washthe organic phase was washed with water
4. extractionThe water phase was back extracted with DCM
5. extractionthe mixture was further extracted with DCM
6. dry with materialdried (Na2SO4)
7. customevaporated under reduced pressure