反应详情

To a solution of N2-(3-fluorophenyl)-5-iodo-N4-propylpyrimidine-2,4-diamine (F2, 2.50 g), bis(triphenylphosphine)palladium(II) dichloride (472 mg) and copper(I) iodide (256 mg) in N,N-dimethylformamide (60 mL), triethylamine (4.7 mL) and N-(4-pentynyl)phthalimide (2.15 g) were added at room temperature, and the mixture was stirred at the same temperature for 2 hours. To the reaction mixture, water and ethyl acetate were added. The organic layer was separated, and the aqueous layer was extracted with ethyl acetate. The organic layer and the extract were combined, washed successively with water, saturated aqueous ammonium chloride and saturated aqueous sodium chloride, and then dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. To the obtained residue, hexane and ethyl acetate were added. The solid matter was taken by filtration, and dried under reduced pressure to obtain 2-(5-(2-((3-fluorophenyl)amino)-4-(propylamino)pyrimidin-5-yl)-4-pentyn-1-yl)isoindoline-1,3-dione (F3, 1.44 g) as yellow solid.

1. customThe organic layer was separated
2. extractionthe aqueous layer was extracted with ethyl acetate
3. washwashed successively with water, saturated aqueous ammonium chloride and saturated aqueous sodium chloride
4. dry with materialdried over anhydrous magnesium sulfate
5. customthe solvent was evaporated under reduced pressure
6. additionTo the obtained residue, hexane and ethyl acetate were added
7. filtrationThe solid matter was taken by filtration
8. customdried under reduced pressure