反应详情

N-(4,4-Dimethyl-1,2,3,4-tetrahydro-isoquinolin-7-yl)-2-[(1H-pyrrolo[2,3-b]pyridin-6-ylmethyl)-amino]-nicotinamide (0.100 g, 0.235 mmol, Example 1), HOAc (Gracious, 0.025 mL, 0.42 mmol), TBTU (0.094 g, 0.293 mmol), DIEA (0.04 mL, 0.23 mmol) were dissolved into 5 mL of DMF and stirred at RT for 1 h. 50 mL of EtOAc was added and the organic phase was washed with 10% Na2CO3 and brine. Then the organic phase was dried over Na2SO4, filtered, and concentrated to give a white solid. The solid was washed with CH3CN, then purified by HPLC (Beckman) to afford the title compound. MS (ES+): 469 (M+H). Calc'd. for C27H28N6O2—468.56.

1. washthe organic phase was washed with 10% Na2CO3 and brine
2. dry with materialThen the organic phase was dried over Na2SO4
3. filtrationfiltered
4. concentrationconcentrated
5. customto give a white solid
6. washThe solid was washed with CH3CN
7. custompurified by HPLC (Beckman)