Hydrochloric Acid → 4-Methoxybicyclo(2.2.2)octane-1-carboxylic acid
反応式
[CH3:1][O:2][C:3]12[CH2:10][CH2:9][C:6]([C:11]([O:13]C)=[O:12])([CH2:7][CH2:8]1)[CH2:5][CH2:4]2.Cl>[OH-].[Na+]>[CH3:1][O:2][C:3]12[CH2:10][CH2:9][C:6]([C:11]([OH:13])=[O:12])([CH2:5][CH2:4]1)[CH2:7][CH2:8]2参加物
4
実験手順
Methyl 4-methoxybicyclo[2.2.2]octane-1-carboxylate (6.5 g, 33 mmol) was refluxed in aqueous sodium hydroxide solution (5%, 150 mL) for 2 h. After cooling down, the reaction solution was acidified with hydrochloric acid solution (6 N, 50 mL) and extracted with ethyl acetate (100 mL×2). The combined organic layers were dried over magnesium sulfate and concentrated to afford the title compound (5.9 g, 32 mmol, yield 97%) which was used in the next step without further purification. MS (ESI) m/z=183.2 [M+H]−.
後処理
- temperatureAfter cooling down
- extractionextracted with ethyl acetate (100 mL×2)
- dry with materialThe combined organic layers were dried over magnesium sulfate
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-05a9d595841344fcb9ff585309138733
- 出典データセット
- uspto-grants-2015_09
- 特許番号
- US09139534B2
反応ノート
読み込み中…