反应详情

温度

60 °C

To 0.5 L flask charged with 5-Bromo-2-chloronicotinic acid (25.0 g, 106.4 mmol) in MeOH (250 mL) was added H2SO4 (5 mL). The mixture was heated to 60° C., stirred for 1.5 day. LC-MS indicated full conversion of starting material at this time. The reaction was cooled to RT and the volatile components removed in vacuo. The crude residue was dissolved in EtOAc (300 mL), quenched with sat. aqueous Na(HCO3)2 (200 mL). The organic layer was separated, washed with brine, dried over MgSO4 and concentrated to afford the compound, methyl-5-bromo-2-chloronicotinate, as a while solid (quantitative yield). LC-MS (M+H)=250.1.

1. temperatureThe reaction was cooled to RT
2. customthe volatile components removed in vacuo
3. dissolutionThe crude residue was dissolved in EtOAc (300 mL)
4. customquenched with sat. aqueous Na(HCO3)2 (200 mL)
5. customThe organic layer was separated
6. washwashed with brine
7. dry with materialdried over MgSO4
8. concentrationconcentrated