Water → 1-Acenaphtheneacetic acid
反応式
C([O:3][C:4](=[O:18])[CH2:5][CH:6]1[C:16]2=[C:17]3[C:12](=[CH:13][CH:14]=[CH:15]2)[CH:11]=[CH:10][CH:9]=[C:8]3[CH2:7]1)C.[OH-].[K+].O>CO>[CH:6]1([CH2:5][C:4]([OH:18])=[O:3])[C:16]2=[C:17]3[C:12](=[CH:13][CH:14]=[CH:15]2)[CH:11]=[CH:10][CH:9]=[C:8]3[CH2:7]1参加物
5
実験手順
The ester obtained in Step C (1.9 g, 7.91.10−3 mol) is heated at reflux in the presence of potassium hydroxide (2.34 g, 4.17.10−2 mol, 5.3 eq.), water (16 ml) and methanol (16 ml) for one night. After evaporating off the solvent, the residue is taken up in water and extracted twice with ether. The basic aqueous phase is acidified using concentrated HCl in the cold state. The acid is extracted with ethyl acetate and dried over MgSO4. After evaporating off the solvent under reduced pressure, the title compound is obtained in the form of a yellow solid.
後処理
- customAfter evaporating off the solvent
- extractionextracted twice with ether
- extractionThe acid is extracted with ethyl acetate
- dry with materialdried over MgSO4
- customAfter evaporating off the solvent under reduced pressure
出典と根拠
- ORDレコード
- ord-05a60df93b1e44c8a9252e7aa4a4a5a4
- 出典データセット
- uspto-grants-2002_07
- 特許番号
- US06423870B1
反応ノート
読み込み中…