Hydrochloric Acid → Methyl 4-chloro-2-hydroxybenzoate
反応式
Cl.[Cl:2][C:3]1[CH:4]=[C:5]([OH:12])[C:6](=[CH:10][CH:11]=1)[C:7]([OH:9])=[O:8].[CH3:13]O>>[Cl:2][C:3]1[CH:4]=[C:5]([OH:12])[C:6](=[CH:10][CH:11]=1)[C:7]([O:9][CH3:13])=[O:8]参加物
4
実験手順
Hydrogen chloride gas is bubbled into a mixture of 4-chlorosalicylic acid (100 g, 0.579 mol) in methanol while maintaining the temperature at 45°-50° C. The reaction mixture is then stirred at room temperature for several hours, concentrated in vacuo and extracted with ether. The combined organic extracts are washed sequentially with brine, saturated sodium hydrogen carbonate solution and brine, dried over anhydrous sodium sulfate and concentrated in vacuo to obtain an amber oil. The oil is distilled under reduced pressure to give the title product as a colorless oil which is identified by NMR spectral analyses.
後処理
- temperaturewhile maintaining the temperature at 45°-50° C
- concentrationconcentrated in vacuo
- extractionextracted with ether
- washThe combined organic extracts are washed sequentially with brine, saturated sodium hydrogen carbonate solution and brine
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated in vacuo
- customto obtain an amber oil
- distillationThe oil is distilled under reduced pressure
出典と根拠
- ORDレコード
- ord-1e8dce9651a145ceb2753c779256c78f
- 出典データセット
- uspto-grants-1996_06
- 特許番号
- US05523278
反応ノート
読み込み中…