Phosphorus oxychloride → HCID 58046417, 화합물
반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[N:12][NH:11][C:10](=O)[CH:9]=2)=[CH:4][CH:3]=1.O=P(Cl)(Cl)[Cl:17]>>[Cl:17][C:10]1[N:11]=[N:12][CH:13]=[C:8]([C:5]2[CH:6]=[CH:7][C:2]([F:1])=[CH:3][CH:4]=2)[CH:9]=1참가 물질
3
반응 조건
- 온도
- 110 °C
실험 절차
5-(4-Fluorophenyl)pyridazin-3(2H)-one (2.15 g, 11.3 mmol) was dissolved in POCl3 (133 ml) and the mixture was refluxed at 110° C. for 30 min. The reaction was cooled in an ice bath and slowly quenched with aqueous sodium hydrogen carbonate (200 mL). The mixture was extracted with ethyl acetate (3×200 mL). The combined organics were washed with water and brine, dried over anhydrous MgSO4, filtered, and concentrated under reduced pressure to afford the title compound. 1H NMR (500 MHz, CD3SOCD3) δ 9.67 (d, 1H); 8.28 (d, 1H); 8.07 (dd, 2H); 7.42 (t, 2H).
후처리
- temperatureThe reaction was cooled in an ice bath
- customslowly quenched with aqueous sodium hydrogen carbonate (200 mL)