Acetic Acid → 5-Methoxy-3-methylbenzofuran
反応式
[C:1]([C:4]1[CH:14]=[C:13]([O:15][CH3:16])[CH:12]=[CH:11][C:5]=1[O:6][CH2:7]C(O)=O)(=O)[CH3:2].C(OC(=O)C)(=O)C.C(O)(=O)C>O>[CH3:16][O:15][C:13]1[CH:12]=[CH:11][C:5]2[O:6][CH:7]=[C:1]([CH3:2])[C:4]=2[CH:14]=1参加物
5
反応条件
- 温度
- 110 °C
実験手順
A mixture of (2-acetyl-4-methoxyphenoxy)acetic acid (10.0 g) synthesized above, acetic anhydride (18.3 g) and acetic acid (100 mL) was stirred at 110° C. for 5 hr, poured into water, and the mixture was extracted with ethyl acetate. The extract was washed with saturated aqueous sodium hydrogen carbonate solution and saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (5% ethyl acetate/hexane) to give the title object compound (5.87 g, 81%) as a colorless oil.
後処理
- extractionthe mixture was extracted with ethyl acetate
- washThe extract was washed with saturated aqueous sodium hydrogen carbonate solution and saturated brine
- dry with materialdried over magnesium sulfate
- concentrationconcentrated under reduced pressure
- customThe residue was purified by silica gel column chromatography (5% ethyl acetate/hexane)
出典と根拠
- ORDレコード
- ord-741101901d7541238fe4c451fc6c11a5
- 出典データセット
- uspto-grants-2013_05
- 特許番号
- US08436043B2
反応ノート
読み込み中…