反应详情

温度

110 °C

To a suspension of 7-bromo-1-[(4-methoxybenzyl)amino][1]benzothieno[3,2-c]pyridine-4-carbonitrile (Example 12, Step 9) in DMF (0.1 M) were added the pyridine-3-boronic acid 1,3-propanediol cyclic ester (1.5 equiv), 2 M Na2CO3 (3 equiv) and PdCl2dppf (0.05 equiv). The mixture was heated in the microwave reactor at 110° C. for 10 min. The reaction mixture was partitioned between EtOAc and saturated NaHCO3. The organic phase was separated, dried over MgSO4, filtered, evaporated and purified by flash chromatography (70:30 hexanes/EtOAc to 100% EtOAc) to provide the title compound.

1. customThe reaction mixture was partitioned between EtOAc and saturated NaHCO3
2. customThe organic phase was separated
3. dry with materialdried over MgSO4
4. filtrationfiltered
5. customevaporated
6. custompurified by flash chromatography (70:30 hexanes/EtOAc to 100% EtOAc)