反应详情

温度

118 °C

POCl3 (3.4 mL, 36 mmol) was added dropwise to 5-fluoro-8-methoxy-2-methyl-quinolin-4-ol (0.56 g, 2.7 mmol) at 0° C. The reaction vessel was equipped with a drying tube containing P4O10 and heated to 118° C. for 2 h. The reaction mixture was concentrated in vacuo and partitioned between DCM (30 mL), water (2 mL), and concentrated aqueous NH3 (2 mL). The organic layer was dried over Na2SO4, filtered, and concentrated in vacuo. The residue was purified by flash chromatography on silica gel (elution with EA/DCM 1:15) to give the title compound. MS (m/z): 226.5 [M+H+]

1. customThe reaction vessel was equipped with a drying tube
2. concentrationThe reaction mixture was concentrated in vacuo
3. custompartitioned between DCM (30 mL), water (2 mL), and concentrated aqueous NH3 (2 mL)
4. dry with materialThe organic layer was dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customThe residue was purified by flash chromatography on silica gel (elution with EA/DCM 1:15)