反应详情

(2-Amino-pyridin-3-yl)-pyridin-3-yl-methanone (0.13 g, 0.65 mmol) is dissolved in glacial acetic acid (6 ml). Na2CO3 (0.075 g, 0.72 mmol) is added. After evolution of gas has finished, a solution of bromine (0.025 ml, 0.49 mmol) in acetic acid (3 ml) is added dropwise. Na2CO3 (0.075 g, 0.72 mmol) is added, followed by a second solution of bromine (0.025 ml, 0.49 mmol) in acetic acid (3 ml). The resulting yellow suspension is left to stir for 2 hour. The reaction is quenched by pouring onto ice water (150 ml), and neutralised using NaHCO3. The product is extracted with EtOAc and dried (MgSO4). Concentration in vacuo affords an oil, which is trituatuted with methanol to yield the title compound [M+H]+ 277.

1. waitThe resulting yellow suspension is left
2. customThe reaction is quenched
3. additionby pouring onto ice water (150 ml)
4. extractionThe product is extracted with EtOAc
5. dry with materialdried (MgSO4)
6. concentrationConcentration in vacuo
7. customaffords an oil, which