反应详情

温度

130 °C

To the solution of [3-(2-methanesulfonyl-pyrimidin-4-yl)-1H-pyrazolo[3,4-d]pyrimidin-6-yl]-(2-morpholin-4-yl-ethyl)-amine (from Example 11 supra) (220 mg, 0.54 mmol) and benzyl-amine (70 mg, 0.65 mmol) in DMSO (15 mL) was added DIPEA (84 mg, 0.65 mmol). The mixture was heated at 130° C. with stirring under N2 for 4 hours. The solvent was removed under reduced pressure. The residue was first purified by column chromatography (silica gel, dichloromethane:MeOH, 50:1 to 30:1), then by prep-HPLC. Concentrated HCl was added to the fractions with product and concentrated under reduced pressure to give [3-(2-benzylamino-pyrimidin-4-yl)-1H-pyrazolo[3,4-d]pyrimidin-6-yl]-(2-morpholin-4-yl-ethyl)-amine; hydrochloride. (Yield 40 mg, 17.1%).

1. customThe solvent was removed under reduced pressure
2. customThe residue was first purified by column chromatography (silica gel, dichloromethane:MeOH, 50:1 to 30:1)
3. additionConcentrated HCl was added to the fractions with product
4. concentrationconcentrated under reduced pressure