Phosphorus oxychloride → HCID 57504627, compound

Participants

Reaction Conditions

Reaction Steps

Phosphorus oxychloride (5.10 ml, 54.75 mmol) was added to 1-(4-methylpyridin-3-yl)-1H-pyrazolo[3,4-d]pyrimidin-4-ol (0.622 g, 2.74 mmol). The resulting solution was stirred at 100° C. for 2 hours. The reaction mixture was evaporated. Toluene was added to the residue and the reaction mixture was concentrated. This was repeated to remove excess POCl3. The residue was dissolved in DMF (15 mL) and MP carbonate was added (˜3 g) and allowed to stir overnight. The DMF was evaporated in vacuo to afford crude product which was used without further purification. 1H NMR (400 MHz, DMSO) δ 2.1 (3H, s), 7.60 (1H, d), 8.65 (1H, d), 8.68 (1H, s), 8.82 (1H, s), 8.91 (1H, s); m/z (ES+) (M+H)+=246; HPLC tR=1.69 min.

Provenance & Evidence