Lithium Hydroxide → 5-Chloro-3-(trifluoromethyl)-1-benzothiophene-2-carboxylic acid
反応式
[Cl:1][C:2]1[CH:18]=[CH:17][C:5]2[S:6][C:7]([C:13]([O:15]C)=[O:14])=[C:8]([C:9]([F:12])([F:11])[F:10])[C:4]=2[CH:3]=1.[Li+].[OH-]>C1COCC1.CO.O>[Cl:1][C:2]1[CH:18]=[CH:17][C:5]2[S:6][C:7]([C:13]([OH:15])=[O:14])=[C:8]([C:9]([F:12])([F:11])[F:10])[C:4]=2[CH:3]=1参加物
4
実験手順
A mixture of compound 11e (390 mg, 1.33 mmol) and LiOH (159 mg, 6.65 mmol) in THF/MeOH/H2O (4/4/4 mL) was stirred for 4 h. The reaction was concentrated under reduced pressure and then water was added to the residue. The aqueous mixture was acidified with 1N HCl to pH ˜4. A white precipitate was filtered and washed with water and Et2O. The crude product was dried under vacuum to give compound 11f which was used without purification.
後処理
- concentrationThe reaction was concentrated under reduced pressure
- additionwater was added to the residue
- filtrationA white precipitate was filtered
- washwashed with water and Et2O
- dry with materialThe crude product was dried under vacuum
出典と根拠
- ORDレコード
- ord-e9ef8874be88478c8fa218fbd79bf920
- 出典データセット
- uspto-grants-2013_11
- 特許番号
- US08575363B2
反応ノート
読み込み中…