Boron tribromide → 5-Hydroxybenzofuran-2-carboxylic acid
反応式
C[O:2][C:3]1[CH:4]=[CH:5][C:6]2[O:10][C:9]([C:11]([OH:13])=[O:12])=[CH:8][C:7]=2[CH:14]=1.B(Br)(Br)Br.[NH4+].[Cl-]>C(Cl)Cl>[OH:2][C:3]1[CH:4]=[CH:5][C:6]2[O:10][C:9]([C:11]([OH:13])=[O:12])=[CH:8][C:7]=2[CH:14]=1参加物
5
実験手順
To a cooled (−78° C.) solution of 5-methoxy-benzofuran-2-carboxylic acid (5.0 g, 26.0 mmol) in DCM (100 mL) was added BBr3 (7.4 mL, 19.5 g, 78.0 mmol) and the reaction mixture was stirred (2 h). The reaction mixture was warmed (rt) and subsequently cooled (0° C.) and treated with saturated NH4Cl (100 mL). The resultant biphasic mixture was partitioned and the aqueous layer was extracted with EtOAc (3×100 mL), dried, filtered and concentrated in vacuo to afford the title compound (4.6 g, 100%).
後処理
- temperaturesubsequently cooled (0° C.)
- customThe resultant biphasic mixture was partitioned
- extractionthe aqueous layer was extracted with EtOAc (3×100 mL)
- customdried
- filtrationfiltered
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-d948c84e079a41c683802ec4cebab464
- 出典データセット
- uspto-grants-2013_03
- 特許番号
- US08399465B2
反応ノート
読み込み中…