Hydrochloric Acid → 4-Chloro-3-(hydroxymethyl)phenol
反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[Cl:7][C:8]1[CH:16]=[CH:15][C:14]([OH:17])=[CH:13][C:9]=1[C:10](O)=[O:11].Cl>O1CCCC1.O.O1CCCC1>[Cl:7][C:8]1[CH:16]=[CH:15][C:14]([OH:17])=[CH:13][C:9]=1[CH2:10][OH:11]参加物
6
実験手順
Lithium aluminium hydride (1M in diethyl ether, 25 mL, 25 mmol) was added to an ice-cooled solution of 2-chloro-5-hydroxy-benzoic acid (4 g, 23.2 mmol) in tetrahydrofuran (200 mL) and the mixture was heated under reflux for 6 hours. The mixture was then diluted with a mixture of water/tetrahydrofuran, acidified with 1M hydrochloric acid, and extracted with ethyl acetate. The organic solution was dried over sodium sulphate and concentrated in vacuo to afford the title compound in quantitative yield, 4.3 g.
後処理
- temperaturethe mixture was heated
- temperatureunder reflux for 6 hours
- extractionextracted with ethyl acetate
- dry with materialThe organic solution was dried over sodium sulphate
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-9d324e7d830b4262a401a8f0f3f35f71
- 出典データセット
- uspto-grants-2011_12
- 特許番号
- US08076356B2
反応ノート
読み込み中…