反应详情

温度

130 °C

3,6-Dichloropyridazine (160 mg, 1.07 mmol) and difluoro-quinolin-6-yl-acetic acid hydrazide (254 mg, 1.07 mmol) were added in n-BuOH (20 mL). The reaction mixture was heated at 130° C. for 12 h. The solvent was removed under reduced pressure. The crude was partitioned in aqueous solution of K2CO3 and EtOAc. The organic layers were combined and concentrated to give a solid, which was purified by silica gel column to give the title compound as black solid (190 mg, 53%). 1H-NMR (400 MHz, DMSO-d6) δ ppm 7.62 (m, 2H), 7.90 (m, 1H), 8.22 (m, 1H), 8.35 (m, 1H), 8.65 (m, 2H), 9.02 (m, 1H).

1. customThe solvent was removed under reduced pressure
2. customThe crude was partitioned in aqueous solution of K2CO3 and EtOAc
3. concentrationconcentrated
4. customto give a solid, which
5. customwas purified by silica gel column