Sulfuric Acid → 2,5-Dichloro-4-sulfanylphenol
反応式
[Cl:1][C:2]1[CH:7]=[C:6]([OH:8])[C:5]([Cl:9])=[CH:4][C:3]=1[S:10](Cl)(=O)=O.OS(O)(=O)=O>[Zn].C1(C)C=CC=CC=1>[Cl:9][C:5]1[CH:4]=[C:3]([SH:10])[C:2]([Cl:1])=[CH:7][C:6]=1[OH:8]参加物
5
反応条件
- 温度
- 120 °C
実験手順
To a mixture of 2,5-dichloro-4-hydroxy-benzenesulfonyl chloride (1.28 g, 4.92 mmol) and a solution of 25% of H2SO4 (17 mL), Zinc dust (1.64 g, 24.56 mmol) was added slowly at room temperature. The reaction mixture was allowed to stir at 120° C. overnight. The mixture was then cooled at room temperature and toluene was added. The layers were separated and the aqueous phase was dried over, MgSO4 filtered and concentrated in vacuo to give 514 mg (54%) of the title compound as a white solid, which was used in the next reaction without further purification.
後処理
- temperatureThe mixture was then cooled at room temperature
- customThe layers were separated
- dry with materialthe aqueous phase was dried over, MgSO4
- filtrationfiltered
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-97109a784b9c43949ddb48c4d4df10b4
- 出典データセット
- uspto-grants-2006_12
- 特許番号
- US07148236B2
反応ノート
読み込み中…