反应详情

温度

100 °C

To a 25 mL flask was added a stir bar, 2-Chloro-7-methylquinoline-6-carbonitrile (0.2 g, 0.98 mmol), Pd2 dba3 (0.11 g, 0.19 mmol), Xantphos (0.090 g, 0.090 mmol), Cesium Carbonate (0.26 g, 0.63 mmol) and tert-Butyl 3-oxopiperazine-1-carboxylate (0.29 g, 1.4 mmol). The resulting mixture was degassed and purged with N2 three times. To the flask was added 1,4-dioxane (4 mL). The reaction mixture was then refluxed at 100° C. overnight. The solution was concentrated in vacuo and the resulting crude was dissolved in EtOAc and washed with brine, dried over Na2SO4, filtered and concentrated in vacuo. The crude residue was then purified by silica gel column chromatography (10% MeOH in DCM) to provide the title compound.

1. additionTo a 25 mL flask was added a stir bar
2. customThe resulting mixture was degassed
3. custompurged with N2 three times
4. additionTo the flask was added 1,4-dioxane (4 mL)
5. concentrationThe solution was concentrated in vacuo
6. dissolutionthe resulting crude was dissolved in EtOAc
7. washwashed with brine
8. dry with materialdried over Na2SO4
9. filtrationfiltered
10. concentrationconcentrated in vacuo
11. customThe crude residue was then purified by silica gel column chromatography (10% MeOH in DCM)