反应详情

温度

180 °C

Treat a solution of 5-bromo-2-fluoropyridine-3-carboxaldehyde (0.50 g, 2.451 mmol) and 1-methylguanidine hydrochloride (0.322 g, 2.94 mmol) in acetonitrile (20 mL) with TEA (0.947 mL, 7.35 mmol) and heat to 180° C. in the microwave for 15 min. Concentrate the mixture to dryness, treat the residue with DCM and wash with H2O, then brine. Dry the organic layer over Na2SO4, concentrate to dryness and purify via silica gel chromatography (20-100% EtOAc/Hexanes) to afford the title compound (140 mg, 24% yield). MS (m/z): 241.0 (M+1).

1. concentrationConcentrate the mixture to dryness
2. additiontreat the residue with DCM
3. washwash with H2O
4. dry with materialDry the organic layer over Na2SO4
5. concentrationconcentrate to dryness
6. custompurify via silica gel chromatography (20-100% EtOAc/Hexanes)