反应详情

A mixture of 4-(1-(4-methoxybenzyl)-3-iodo-1H-pyrazolo[3,4-b]pyridin-4-yloxy)-3-fluorobenzenamine (0.10 g, 0.20 mmol; prepared as in Example 7, Step B), 1-methylpiperidin-4-amine (0.070 g, 0.61 mmol), (S)-pyrrolidine-2-carboxylic acid (9.4 mg, 0.82 mmol), CuI (7.8 mg, 0.041 mmol), and K2CO3 (0.14 g, 1.0 mmol) was heated in DMSO (4 mL) with sealed tube at 100° C. for 17 hours. The reaction mixture was cooled to ambient temperature and treated with CH2Cl2, washed with water, dried over MgSO4, and concentrated to give crude material which was purified by silica gel flash column chromatography (10% MeOH in CH2Cl2) to afford 49 mg (50%) of the desired product. LRMS (ESI pos) m/e 477.1 (M+1).

1. customwith sealed tube at 100° C. for 17 hours
2. washwashed with water
3. dry with materialdried over MgSO4
4. concentrationconcentrated
5. customto give crude material which
6. customwas purified by silica gel flash column chromatography (10% MeOH in CH2Cl2)