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