反应详情

TFA (1.0 mL, 13 mmol) was added drop-wise over about 1 min to a 100 mL round-bottomed flask containing a solution of tert-butyl-cis-4-((6-(4-methyl-3-sulfamoylphenylamino)-1H-pyrazolo[3,4-d]pyrimidin-1-yl)methyl)cyclohexylcarbamate (0.55 g, 1.1 mmol, Example #B.1.1) in DCM (5 mL) at ambient temperature. The reaction mixture was allowed to stir for about 2 h then concentrated under reduced pressure. The crude product was purified by RP-HPLC (Table 2, Method b) to give 5-(1-((cis-4-aminocyclohexyl)methyl)-1H-pyrazolo[3,4-d]pyrimidin-6-ylamino)-2-methylbenzenesulfonamide (0.435 g. 95%) as a white solid. LC/MS (Table 2, Method a) Rt=1.39 min; MS m/z: 414 (M+H)+.

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