Phosphorus oxychloride → HCID 57465578, 화합물
반응식
[CH3:1][C:2]1[C:6]([C:7]2[CH:16]=[C:15]3[C:10]([C:11](O)=[C:12]([N+:17]([O-:19])=[O:18])[CH:13]=[N:14]3)=[CH:9][CH:8]=2)=[C:5]([CH3:21])[O:4][N:3]=1.O=P(Cl)(Cl)[Cl:24]>>[Cl:24][C:11]1[C:10]2[C:15](=[CH:16][C:7]([C:6]3[C:2]([CH3:1])=[N:3][O:4][C:5]=3[CH3:21])=[CH:8][CH:9]=2)[N:14]=[CH:13][C:12]=1[N+:17]([O-:19])=[O:18]참가 물질
3
실험 절차
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).
후처리
- temperaturewas refluxed overnight
- temperatureAfter cooling the solvent
- customwas evaporated in vacuo