Phosphorus oxychloride → 4-Chloro-6-fluoroquinoline
反応式
[F:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[CH:7][CH:6]=[C:5]2O.P(Cl)(Cl)([Cl:15])=O>>[Cl:15][C:5]1[C:4]2[C:9](=[CH:10][CH:11]=[C:2]([F:1])[CH:3]=2)[N:8]=[CH:7][CH:6]=1参加物
3
実験手順
A mixture of 52 g (0.319 mol) of 6-fluoro-4-hydroxyquinoline and 100 ml of phosphorus oxychloride was stirred and heated under reflux for 3 hr. The reaction mixture was concentrated in vacuo. A slurry of the residue in methylene chloride was poured into ice-water, and the mixture neutralized with 3N sodium hydroxide. The organic phase was separated, and the aqueous phase was extracted with 250 ml of methylene chloride twice. The organic phases were combined, washed with water, dired over sodium sulfate, and concentrated in vacuo. The residue was crystallized from hexane to give 27.95 g of product, mp 71°-74°.
後処理
- temperatureheated
- temperatureunder reflux for 3 hr
- concentrationThe reaction mixture was concentrated in vacuo
- additionA slurry of the residue in methylene chloride was poured into ice-water
- customThe organic phase was separated
- extractionthe aqueous phase was extracted with 250 ml of methylene chloride twice
- washwashed with water
- concentrationconcentrated in vacuo
- customThe residue was crystallized from hexane
出典と根拠
- ORDレコード
- ord-9246968d547d49439aba6f2b4f69d835
- 出典データセット
- uspto-grants-1985_12
- 特許番号
- US04560692
反応ノート
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