Lithium Hydroxide → 2-Chloro-4-methylbenzoic acid
反応式
[Cl:1][C:2]1[CH:11]=[C:10]([CH3:12])[CH:9]=[CH:8][C:3]=1[C:4]([O:6]C)=[O:5].[OH-].[Li+]>O1CCCC1.O>[Cl:1][C:2]1[CH:11]=[C:10]([CH3:12])[CH:9]=[CH:8][C:3]=1[C:4]([OH:6])=[O:5]参加物
5
反応条件
- 温度
- 50 °C
実験手順
To methyl 2-chloro-4-methylbenzoate (1.00 g, 5.42 mmol) in tetrahydrofuran (10 mL) methyl alcohol (5 mL) and water (2.5 mL) is added 2N lithium hydroxide (8.12 mL, 16.2 mmol). The reaction mixture is heated at 50° C. for 2.5 hr, cooled to room temperature, and then quenched with 5N hydrochloric acid (3.24 mL). The mixture is concentrated to remove the tetrahydrofuran and methyl alcohol. A white precipitate is formed and is filtered. After drying, 0.922 g (100%) of 2-chloro-4-methylbenzoic acid is isolated. ES(−)MS m/z 169, (M−H)− consistent with 1 Cl.
後処理
- temperaturecooled to room temperature
- customquenched with 5N hydrochloric acid (3.24 mL)
- concentrationThe mixture is concentrated
- customto remove the tetrahydrofuran and methyl alcohol
- customA white precipitate is formed
- filtrationis filtered
- customAfter drying
出典と根拠
- ORDレコード
- ord-cea61636641643349db50d2479857ff0
- 出典データセット
- uspto-grants-2006_08
- 特許番号
- US07084170B2
反応ノート
読み込み中…