反应详情

温度

0 °C

4-(7-(cyclopropylamino)pyrazolo[1,5-a]pyrimidin-5-ylamino)benzonitrile hydrochloride (205 mg, 0.62 mmol) was dissolved in anhydrous DMF (1 mL) and the solution was cooled to 0° C. by an external ice bath. POCl3 (115 μL, 1.25 mmol) was added dropwise keeping the internal temperature <5° C. After addition, the ice bath was removed. After 5 h, the solution was poured into H2O (20 mL) and the pH was adjusted to 11 by the addition of 6N NaOH. The solution was allowed to stir for 1 h, and the precipitate was filtered off. The crude product was triturated with EtOH (7 mL), filtered, and dried under high vacuum (1 mmHg) to provide 4-(7-(cyclopropylamino)-3-formylpyrazolo[1,5-a]pyrimidin-5-ylamino)benzonitrile (129 mg, 64%) as an orange solid. LCMS (ES): >90% pure, m/z 319 [M+1]+.

1. customthe internal temperature <5° C
2. additionAfter addition
3. customthe ice bath was removed
4. additionthe solution was poured into H2O (20 mL)
5. additionthe pH was adjusted to 11 by the addition of 6N NaOH
6. filtrationthe precipitate was filtered off
7. customThe crude product was triturated with EtOH (7 mL)
8. filtrationfiltered
9. customdried under high vacuum (1 mmHg)