Lithium hydroxide, monohydrate → 7-Bromo-1-benzofuran-3-carboxylic acid
反応式
[Br:1][C:2]1[C:10]2[O:9][CH:8]=[C:7]([C:11]([O:13]CC)=[O:12])[C:6]=2[CH:5]=[CH:4][CH:3]=1.O[Li].O>CO.C1COCC1.O>[Br:1][C:2]1[C:10]2[O:9][CH:8]=[C:7]([C:11]([OH:13])=[O:12])[C:6]=2[CH:5]=[CH:4][CH:3]=1参加物
4
実験手順
To a solution of ethyl 7-bromo-1-benzofuran-3-carboxylate (1.0 g, 3.7 mmol) in 20 mL of MeOH/THF/H2O (2/211) was added LiOH H2O (777 mg, 18.5 mmol), and the mixture was stirred at ambient temperature overnight. The solvents were removed under vacuum, and the residue was added 10 mL of water and extracted with ether (100 mL). The aqueous layer was then acidified with 4 N HCl to pH=3 in ice bath, and extracted with EtOAc. The combined organic phase was washed with brine, dried over anhydrous sodium sulfate and concentrated to give 7-bromo-1-benzofuran-3-carboxylic acid.
後処理
- customThe solvents were removed under vacuum
- additionthe residue was added 10 mL of water
- extractionextracted with ether (100 mL)
- extractionextracted with EtOAc
- washThe combined organic phase was washed with brine
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-c5eef8cc7c504d9ba82c9937127bdd2e
- 出典データセット
- uspto-grants-2015_06
- 特許番号
- US09056859B2
反応ノート
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