反应详情

2-Prop-2-ynyl-1,2,3,4-tetrahydro-isoquinoline (0.72 mmol), 5-bromo-4-(2,2-dimethyl-propylamino)-pyrimidine-2-carbonitrile (0.86 mmol), Bis(benzonitrile)-palladium(II) chloride (0.02 mmol), copper (I) iodide (0.015 mmol), tri-tert-butylphosphine (0.04 mmol) and diisopropyl amine (0.86 mmol) in dioxane (4 ml) is stirred at room temperature for 2.5 h. After filtration, the reaction mixture is treated with saturated ammonium chloride. The mixture is extracted with AcOEt. The organic layer is washed with brine, dried over magnesium sulfate and evaporated down. The crude product is applied to a column of silica gel, which is eluted with following solvents: n-hexane:AcOEt=1:1 (v/v) and n-hexane:AcOEt=1:5 (v/v). The solvent of the latter effluent is removed by evaporation and dried in vacuo afford the title compound. yield 46.5%, Rf=0.31 (n-hexane:AcOEt=1:1).

1. filtrationAfter filtration
2. additionthe reaction mixture is treated with saturated ammonium chloride
3. extractionThe mixture is extracted with AcOEt
4. washThe organic layer is washed with brine
5. dry with materialdried over magnesium sulfate
6. customevaporated down
7. washis eluted with following solvents
8. customThe solvent of the latter effluent is removed by evaporation
9. customdried in vacuo