反应详情

温度

30 °C

N4-(2,2,2-trifluoroethyl)-N2-(1-((2-(trimethylsilyl)ethoxy)methyl)-1H-indazol-6-yl)furo[3,2-d]pyrimidine-2,4-diamine (1.08 g, 2.257 mmol) was dissolved in DCM (15 mL). TFA (10 mL, 130 mmol) was added. The resulting mixture was stirred at about 30° C. for about 6 h. The mixture was concentrated in vacuo. The residue was diluted with DCM (30 mL) and the pH was adjusted to about pH=9.0 with concentrated NH4OH. The solvents were removed under reduced pressure and the resulting mixture was purified by preparative-HPLC (Table 2, method w) to afford N2-(1H-indazol-6-yl)-N4-(2,2,2-trifluoroethyl)furo[3,2-d]pyrimidine-2,4-diamine (0.15 g, 19%): LC/MS (Table 2, Method h) Rt=1.79 min; MS m/z: 349 (M+H)+. Syk IC50=A

1. concentrationThe mixture was concentrated in vacuo
2. additionThe residue was diluted with DCM (30 mL)
3. customThe solvents were removed under reduced pressure
4. customthe resulting mixture was purified by preparative-HPLC (Table 2, method w)