HRID456062

反应详情

EQUATION

反应方程式

HRID 456062 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe solvent was removed by vacuo
  2. extractionThe crude was extracted by the solution of K2CO3 and EtOAc
  3. customThe organic layer was collected
  4. concentrationconcentrated
  5. customto give a solid, which
  6. customwas purified by silica gel column