反应详情

To a stirred mixture of 19 (0.2 g, 0.52 mmol), isonicotinoyl chloride hydrochloride (0.18 g, 1.04 mmol), and cesium carbonate (0.68 g, 2.08 mmol) in acetonitrile (20 ml) was heated to reflux for 16 h. The reaction mixture was quenched with ice water and extracted with CH2Cl2. The combined organic layer was dried over MgSO4 and evaporated to give a residue that was purified by silica gel flash column chromatography (EtOAc:n-hexane :NH3(aq)=3:2:1%) and recrystallized (CH2Cl2/EtOAc) to afford compound 26, yield 82%.

1. temperaturewas heated
2. temperatureto reflux for 16 h
3. customThe reaction mixture was quenched with ice water
4. extractionextracted with CH2Cl2
5. dry with materialThe combined organic layer was dried over MgSO4
6. customevaporated
7. customto give a residue that
8. customwas purified by silica gel flash column chromatography (EtOAc:n-hexane :NH3(aq)=3:2:1%)
9. customrecrystallized (CH2Cl2/EtOAc)