Iodine → 6-Hydroxy-7-iodo-benzothiazole
反応式
[OH:1][C:2]1[CH:10]=[CH:9][C:5]2[N:6]=[CH:7][S:8][C:4]=2[CH:3]=1.[I:11]I.S([O-])([O-])=O.[Na+].[Na+]>CO.O>[OH:1][C:2]1[CH:10]=[CH:9][C:5]2[N:6]=[CH:7][S:8][C:4]=2[C:3]=1[I:11]参加物
5
実験手順
6-Hydroxy-benzothiazole (0.39 g) and iodine (1.32 g) were dissolved in methanol/water (15 ml/5 ml) to prepare a solution which was then stirred at room temperature for 2 days. An aqueous sodium sulfite solution was added to the reaction solution, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was then washed with water and was dried over anhydrous sodium sulfate. The solvent was removed by distillation under the reduced pressure, and the residue was purified by column chromatography using acetone-chloroform to give 6-hydroxy-7-iodo-benzothiazole (211 mg, yield 29%).
後処理
- customto prepare a solution which
- extractionthe mixture was extracted with ethyl acetate
- washThe ethyl acetate layer was then washed with water
- dry with materialwas dried over anhydrous sodium sulfate
- customThe solvent was removed by distillation under the reduced pressure
- customthe residue was purified by column chromatography
出典と根拠
- ORDレコード
- ord-e4ffdf2d0c8043cda58873b24e61dd2a
- 出典データセット
- uspto-grants-2009_07
- 特許番号
- US07560558B2
反応ノート
読み込み中…