反应详情

温度

130 °C

The mixture of 2-[3-(2-methane sulfinyl-pyrimidin-4-yl)-1H-pyrazolo[3,4-d]pyrimidin-6-ylamino]-ethanol (from Example 21 supra) (1.9 g, crude, 2.31 mmol) and 3-chlorobenzylamine (797 mg, 4.62 mmol) was heated at 130° C. with stirring for 3 hours. The solvent was removed under reduced pressure and the solid was purified by prep-TLC and prep-HPLC. Concentrated HCl was added to the fractions with product and concentrated under reduced pressure to give 2-{3-[2-(3-chloro-benzylamino)-pyrimidin-4-yl]-1H-pyrazolo[3,4-d]pyrimidin-6-ylamino}-ethanol; hydrochloride. (Yield 28 mg, 3.1% of the 3 steps).

1. customThe solvent was removed under reduced pressure
2. customthe solid was purified by prep-TLC and prep-HPLC
3. additionConcentrated HCl was added to the fractions with product
4. concentrationconcentrated under reduced pressure