反应详情

A suspension of 7-(3,5-dimethyl-4-isoxazolyl)-6-(methoxy)-3-nitro-4-quinolinol (for a preparation see Intermediate 17, 5 g, 16 mmol) in POCl3 (20 ml) was refluxed overnight. After cooling, the mixture was evaporated to dryness. The resulting residue was poured over saturated aqueous Sodium hydrogen carbonate and extracted with DCM. The organic layer was washed with water, dried over Na2SO4. The solvent was evaporated under reduce pressure to give the title compound as a light brown powder (5 g, 94%). 1H NMR (300 MHz, DMSO-d6, ppm) δ: 9.27 (s, 1H), 8.15 (s, 1H), 7.73 (s, 1H), 4.05 (s, 3H), 2.36 (s, 3H), 2.16 (s, 3H).

1. temperaturewas refluxed overnight
2. temperatureAfter cooling
3. customthe mixture was evaporated to dryness
4. additionThe resulting residue was poured over saturated aqueous Sodium hydrogen carbonate
5. extractionextracted with DCM
6. washThe organic layer was washed with water
7. dry with materialdried over Na2SO4
8. customThe solvent was evaporated