反应详情

温度

160 °C

To a 2-5 ml Personal Chemistry microwave vial was added 2-(quinolin-6-yl)propanoic acid (0.25 g, 1.2 mmol), 1-(6-phenylpyridazin-3-yl)hydrazine (0.42 g, 2.2 mmol) and conc. HCl (2 mL). The mixture was heated in the microwave at 160° C. for 8 h. After cooling to rt, the mixture was poured into sat. NaHCO3 (100 mL) and then extracted with EtOAc (4×75 mL). The combined extracts were washed with brine, dried (Na2SO4) and concentrated onto silica. Purification by silica gel chromatography (1.0 to 4.5% MeOH (2 M in NH3)/CH2Cl2) afforded the title compound as an off-white solid (0.23 g, 53% yield). MS (ESI, pos. ion) m/z: 352 (M+1).

1. temperatureAfter cooling to rt
2. extractionextracted with EtOAc (4×75 mL)
3. washThe combined extracts were washed with brine
4. dry with materialdried (Na2SO4)
5. concentrationconcentrated onto silica
6. customPurification by silica gel chromatography (1.0 to 4.5% MeOH (2 M in NH3)/CH2Cl2)