Phosphorus oxychloride → 4-Chloro-5,8-difluoro-2-methyl-quinoline
反応式
O[C:2]1[C:11]2[C:6](=[C:7]([F:13])[CH:8]=[CH:9][C:10]=2[F:12])[N:5]=[C:4]([CH3:14])[CH:3]=1.P(Cl)(Cl)([Cl:17])=O>>[Cl:17][C:2]1[C:11]2[C:6](=[C:7]([F:13])[CH:8]=[CH:9][C:10]=2[F:12])[N:5]=[C:4]([CH3:14])[CH:3]=1参加物
3
実験手順
4-Hydroxy-5,8-difluoro-2-methylquinoline (5.4 g) in phosphoryl chloride (60 ml) was boiled for 4 h. The mixture was cooled to room temperature, excess phosphoryl chloride removed at reduced pressure, the residue dissolved in ethyl acetate, washed with sodium hydrogen carbonate, dried (Na2SO4) and solvent removed at reduced pressure. The title compound (5.35 g) was isolated as a brown powder. (Method B). 1H NMR δ: 2.61 (3H, s), 7.46 (1H, m), 7.66 (1H, m), 7.81 (1H, s).
後処理
- customexcess phosphoryl chloride removed at reduced pressure
- dissolutionthe residue dissolved in ethyl acetate
- washwashed with sodium hydrogen carbonate
- dry with materialdried (Na2SO4) and solvent
- customremoved at reduced pressure
出典と根拠
- ORDレコード
- ord-4b454f3f65ed464db04cba23baf9e15b
- 出典データセット
- uspto-grants-2004_03
- 特許番号
- US06699879B1
反応ノート
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