反应详情

0.6 g (1.94 mmol) of the compound obtained in Step 3 of Example 1 and 0.75 g (3.88 mmol) of 5-(4-methylpiperazin-1-yl)piridin-2-amine were dissolved in 8 ml of 1,4-dioxane, and 178 mg (0.2 mmol) of tris(dibenzylideneacetone)dipalladium(O) and 122 mg (0.2 mmol) of 2,2′-bis(diphenylphosphino)-1,1′-binaphthy were added thereto, and stirred for 5 minutes at room temperature. 1.27 g (3.88 mmol) of cesium carbonate was added thereto, and stirred for 3 hours at 100° C. Upon the completion of the reaction, the resulting mixture was cooled to room temperature and filtered over a short bed of Celite filter, and diluted with dichloromethane and washed with water. The organic layer was separated, dried over anhydrous Na2SO4, and filtered and distilled under a reduced pressure. The resulting residue was separated by column chromatography (dichloromethane:methanol (20:1, v/v)) to obtain 630 mg of the title compound (yield: 70%).

1. stirringstirred for 3 hours at 100° C
2. customUpon the completion of the reaction
3. temperaturethe resulting mixture was cooled to room temperature
4. filtrationfiltered over a short bed of Celite
5. filtrationfilter
6. additiondiluted with dichloromethane
7. washwashed with water
8. customThe organic layer was separated
9. dry with materialdried over anhydrous Na2SO4
10. filtrationfiltered
11. distillationdistilled under a reduced pressure
12. customThe resulting residue was separated by column chromatography (dichloromethane:methanol (20:1