反应详情

To a solution N2-{5-[5-(amino)-1-{[2-(trimethylsilyl)ethoxy]methyl}-1H-pyrrolo[2,3-b]pyridin-3-yl]pyridin-3-yl}-N-(2,2,2-trifluoroethyl)valinamide 5-1b (50 mg, 0.093 mmol) in DCM (2 mL) was added TFA (1.4 mL, 18.6 mmol) and the resultant mixture was stirred for 2 h. The mixture was concentrated in vacuo, resuspended in MeOH (1 mL) and to this was added ethylenediamine (13 μl, 0.186 mmol) and sodium hydroxide (10 M aq) (0.065 mL, 0.652 mmol). After 18 h, the reaction was transferred to vial with an additional 1 mL of dimethylsulfoxide and this solution was purified by mass triggered reverse phase HLPC. The fractions containing product 5-1 were basified with NaHCO3, dried over MgSO4, filtered and concentrated. MS APCI: [M+H]+ m/z=407.1.

1. concentrationThe mixture was concentrated in vacuo
2. customthis solution was purified by mass triggered reverse phase HLPC
3. additionThe fractions containing product 5-1
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated