Methanol → Methyl 3-ethylbenzoate
反応式
OS(O)(=O)=O.[CH2:6]([C:8]1[CH:9]=[C:10]([CH:14]=[CH:15][CH:16]=1)[C:11]([OH:13])=[O:12])[CH3:7].[CH3:17]O>O>[CH2:6]([C:8]1[CH:9]=[C:10]([CH:14]=[CH:15][CH:16]=1)[C:11]([O:13][CH3:17])=[O:12])[CH3:7]参加物
5
実験手順
Concentrated H2SO4 (1.0 mL) was added to a solution of 3-ethylbenzoic acid (500 mg, 3.33 mmol) in MeOH (10 mL). The mixture was heated at reflux for 18 h then cooled to room temperature. The mixture was diluted with water (50 mL) and extracted with Et2O (3×100 mL). The combined organic phase was dried (Na2SO4), filtered and concentrated in vacuo. Purification of the crude residue by chromatography on silica gel (hexanes→20% EtOAc/hexanes, gradient) afforded 500 mg (91%) of methyl 3-ethylbenzoate.
後処理
- temperatureThe mixture was heated
- temperatureat reflux for 18 h
- extractionextracted with Et2O (3×100 mL)
- dry with materialThe combined organic phase was dried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated in vacuo
- customPurification of the crude residue by chromatography on silica gel (hexanes→20% EtOAc/hexanes, gradient)
出典と根拠
- ORDレコード
- ord-2d3725fd1f9a4187a86fa47cc24da609
- 出典データセット
- uspto-grants-2013_11
- 特許番号
- US08592413B2
反応ノート
読み込み中…