反应详情

2-{[4-({3-chloro-4-[(3-fluorobenzyl)oxy]phenyl}amino)-1H-pyrazolo[3,4-d]pyrimidin-3-yl]oxy}ethanol (prepared as described in Example 1/550 mg, 1.28 mmol) was dissolved in thionyl chloride (4 ml). DMF (20 μl) was added and the mixture refluxed for 2 hours under a dry atmosphere. After evaporation of the solvent under reduced pressure, the solid residue was triturated in ether, filtered and dried under vacuum to provide the title compound as a hydrochloride salt (551 mg, 89%); NMR Spectrum: 4.03 (t, 2H), 4.58 (t, 2H), 5.28 (s, 2H), 7.18 (t, 1H), 7.29-7.34 (m, 3H), 7.45-7.53 (m, 2H), 7.83 (s, 1H), 8.32 (s, 1H), 9.25 (br s, 1H).

1. temperaturethe mixture refluxed for 2 hours under a dry atmosphere
2. customAfter evaporation of the solvent under reduced pressure
3. customthe solid residue was triturated in ether
4. filtrationfiltered
5. customdried under vacuum