反应详情

A mixture of potassium acetate (13 g, 130 mmol), PdCl2(P-t-Bu2Ph)2 (1.1 g, 1.7 mmol), 4-chloro-1H-pyrazolo[3,4-d]pyrimidine (6.70 g, 43 mmol) and 2-fluoropyridin-3-ylboronic acid (7.3 g, 52 mmol) in EtOH (300 ml)-water (100 ml) was sonicated until the solid became a fine powder and degassed under vacuum. The mixture was refluxed under N2 overnight. After cooling to rt solvent was removed in vacuo and to the residues was added water (200 ml) and NaHCO3 (sat. 150 ml). The mixture was stirred for 15 min. The solid was filtered and washed with water. The solid was dissolved in MeOH-DCM and preloaded on silica gel and purified by flash chromatography eluting with MeOH/DCM (1-5%) to give 4-(2-fluoropyridin-3-yl)-1H-pyrazolo[3,4-d]pyrimidine. MS Found: (ESI pos. ion) m/z 216 (M+H+).

1. customwas sonicated until the solid
2. customdegassed under vacuum
3. temperatureThe mixture was refluxed under N2 overnight
4. customwas removed in vacuo and to the residues
5. additionwas added water (200 ml) and NaHCO3 (sat. 150 ml)
6. filtrationThe solid was filtered
7. washwashed with water
8. dissolutionThe solid was dissolved in MeOH-DCM
9. custompurified by flash chromatography
10. washeluting with MeOH/DCM (1-5%)