反应详情

温度

100 °C

Phosphoryl trichloride (235 mL, 2455.17 mmol) was added to 1-(3-chloropyridin-2-yl)-1H-pyrazolo[3,4-d]pyrimidin-4-ol B15b (30.4 g, 122.76 mmol). The resulting solution was stirred at 100° C. for 4 hours. The mixture was concentrated in vacuo and to the residue was added an ice/water mixture. The resulting mixture was stirred for 1 hour during which time a solid precipitated. The solid was collected by filtration and washed with water (3×75 mL). The crude product was dissolved in EtOAc (500 mL) and dried over MgSO4, filtered and evaporated to afford 4-chloro-1-(3-chloropyridin-2-yl)-1H-pyrazolo[3,4-d]pyrimidine (28.7 g). 1H NMR (400 MHz, DMSO-d6) δ 7.78 (1H, dd), 8.37 (1H, dd), 8.69 (1H, dd), 8.83 (1H, s), 8.92 (1H, s), m/z (ESI+) (M+H)+=266; HPLC tR=1.72 min.

1. concentrationThe mixture was concentrated in vacuo and to the residue
2. additionwas added an ice/water mixture
3. stirringThe resulting mixture was stirred for 1 hour during which time a solid
4. customprecipitated
5. filtrationThe solid was collected by filtration
6. washwashed with water (3×75 mL)
7. dissolutionThe crude product was dissolved in EtOAc (500 mL)
8. dry with materialdried over MgSO4
9. filtrationfiltered
10. customevaporated