Phosphorus oxychloride → 2-Chloro-6-methoxy-4-methylquinoline
반응식
P(Cl)(Cl)([Cl:3])=O.[CH3:6][O:7][C:8]1[CH:9]=[C:10]2[C:15](=[CH:16][CH:17]=1)[NH:14][C:13](=O)[CH:12]=[C:11]2[CH3:19]>>[CH3:6][O:7][C:8]1[CH:9]=[C:10]2[C:15](=[CH:16][CH:17]=1)[N:14]=[C:13]([Cl:3])[CH:12]=[C:11]2[CH3:19]참가 물질
3
반응 조건
- 온도
- 50 °C
실험 절차
A 1-liter, four necked round bottom flask equipped with a mechanical stirrer, thermowatch, and condenser was charged with 630 grams (383 ml) of phosphorous oxychloride. The solution was heated to 50° C. and 6-methoxy-4-methyl-2-quinolone (2) (164.5 g, 0.87 moles) was added over 20 minutes. The reaction mixture was heated to reflux and held there for 2 hours. The hot reaction mixture was slowly poured into ice water (2.5 liters) and the resulting solution cooled to 30° C. The product was removed by suction filtration, washed with water and air dried to yield the title compound 156 g (86.4%); mp 144-145° C. (Lit2 mp 143.5-144.5° C.);