反应详情

Acetyl chloride (0.027 mL, 0.38 mmol) was added to a 10 mL vial charged with 5-(1-((cis-4-aminocyclohexyl)methyl)-1H-pyrazolo[3,4-d]pyrimidin-6-ylamino)-2-methylbenzenesulfonamide (0.15 g, 0.36 mmol, Example #C.1.1) and TEA (1 mL) in THF (4 mL). The reaction mixture was stirred at ambient temperature for about 2 h, then concentrated under reduced pressure. The crude product was purified by RP-HPLC (Table 2, Method b) to give N-(cis-4-((6-(4-methyl-3-sulfamoylphenylamino)-1H-pyrazolo[3,4-d]pyrimidin-1-yl)methyl)cyclohexyl)acetamide (0.021 g, 13%) as a white solid. LC/MS (Table 2, Method a) Rt=1.71 min; MS m/z: 458 (M+H)+.

1. concentrationconcentrated under reduced pressure
2. customThe crude product was purified by RP-HPLC (Table 2, Method b)