HRID2381081

反应详情

EQUATION

反应方程式

HRID 2381081 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
78 °C

PROCEDURE

实验过程

10% Palladium on carbon (23.96 mg, 0.02 mmol) was added to 6-[4-(1H-indol-3-yl)-5,6-dihydropyridin-1(2H)-yl]-3-(trifluoromethyl)-7,8-dihydro-[1,2,4]triazolo[4,3-b]pyridazine (obtained as described in Example 2) (87 mg, 0.23 mmol) and ammonium formate (71.0 mg, 1.13 mmol) in ethanol (20 mL). The resulting mixture was stirred at 78° C. for 2 hours. The reaction mixture was cooled to room temperature, evaporated to dryness, then re-dissolved in ethyl acetate (25 mL) and the solution washed sequentially with water (20 mL) and saturated brine (10 mL). The organic layer was dried over MgSO4, filtered and evaporated to afford 6-[4-(1H-indol-3-yl)piperidin-1-yl]-3-(trifluoromethyl)-7,8-dihydro[1,2,4]triazolo[4,3-b]pyridazine (60.0 mg, 69%) as a solid.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. customevaporated to dryness
  3. dissolutionre-dissolved in ethyl acetate (25 mL)
  4. washthe solution washed sequentially with water (20 mL) and saturated brine (10 mL)
  5. dry with materialThe organic layer was dried over MgSO4
  6. filtrationfiltered
  7. customevaporated