HRID456062
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 130 °C
PROCEDURE
实验过程
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 to 130° C. for 12 hours. The solvent was removed by vacuo. The crude was extracted by the solution of K2CO3 and EtOAc. The organic layer was collected and concentrated to give a solid, which was purified by silica gel column to give 6-[(6-chloro-[1,2,4]triazolo[4,3-b]pyridazin-3-yl)-difluoro-methyl]-quinoline as a black solid (190 mg, 53%). 1H-NMR (DMSO) 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).
WORKUP
后处理
- customThe solvent was removed by vacuo
- extractionThe crude was extracted by the solution of K2CO3 and EtOAc
- customThe organic layer was collected
- concentrationconcentrated
- customto give a solid, which
- customwas purified by silica gel column