反应详情

A suspension of 7-(3,5-dimethyl-4-isoxazolyl)-3-nitro-4-quinolinol (for a preparation see intermediate 15, 5 g, 17 mmol) in POCl3 (50 ml) was refluxed overnight. After cooling the solvent was evaporated in vacuo. The resulting residue was poured over saturated aqueous Sodium hydrogen carbonate, extracted with DCM, washed with water, dried over Na2SO4. The solvent was evaporated under reduce pressure to give the title compound as a light brown solid (4 g, 75%). 1H NMR (300 MHz, CDCl3, ppm) δ: 9.23 (s, 1H), 8.45 (d, J=8.9 Hz, 1H), 8.04 (d, J=1.5 Hz, 1H), 7.67 (dd, J=8.9, 1.5 Hz, 1H), 2.47 (s, 3H), 2.32 (s, 3H).

1. temperaturewas refluxed overnight
2. temperatureAfter cooling the solvent
3. customwas evaporated in vacuo
4. additionThe resulting residue was poured over saturated aqueous Sodium hydrogen carbonate
5. extractionextracted with DCM
6. washwashed with water
7. dry with materialdried over Na2SO4
8. customThe solvent was evaporated