Hydrochloric Acid → 2-Chloro-4,5-difluorobenzoic acid
反応式
C[C:2]([C:4]1[C:9]([Cl:10])=[CH:8][C:7]([F:11])=[C:6]([F:12])[CH:5]=1)=[O:3].Cl[O-:14].[Na+].Cl>C(Cl)Cl>[Cl:10][C:9]1[CH:8]=[C:7]([F:11])[C:6]([F:12])=[CH:5][C:4]=1[C:2]([OH:3])=[O:14]参加物
5
実験手順
To 19.1 g (0.1 mol) of 2-chloro-4,5-difluoroacetophenone, 280.4 g (0.4 mol) of a 12% sodium hypochlorite aqueous solution was added, and the mixture was reacted under reflux for 4 hours. After cooling, concentrated hydrochloric acid was dropwise added thereto until the pH became 1. The formed white crystals were dissolved in methylene chloride and separated from the aqueous phase. The separated aqueous phase was extracted twice with methylene chloride, and the extracts were added to the oil phase. Then, the solvent was distilled off to obtain 16.4 g (yield: 85.1%) of 2-chloro-4,5-difluorobenzoic acid as white crystal.
後処理
- customthe mixture was reacted
- temperatureunder reflux for 4 hours
- temperatureAfter cooling
- customseparated from the aqueous phase
- extractionThe separated aqueous phase was extracted twice with methylene chloride
- additionthe extracts were added to the oil phase
- distillationThen, the solvent was distilled off
出典と根拠
- ORDレコード
- ord-7033b73d738e4bb29fffa2f01965f0e4
- 出典データセット
- uspto-grants-1991_11
- 特許番号
- US05068449
反応ノート
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