Methanol → 3-Bromo-2-methoxybenzenemethanol
反応式
[BH4-].[Li+].C[O:4][C:5](=O)[C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([Br:12])[C:7]=1[O:13][CH3:14].CO>CCOCC>[Br:12][C:8]1[C:7]([O:13][CH3:14])=[C:6]([CH2:5][OH:4])[CH:11]=[CH:10][CH:9]=1参加物
5
実験手順
2.4 g of lithium borohydride (LiBH4) was added to a solution of 5.3 g of 3-bromo-2-methoxy-benzoic acid methyl ester 5 in 200 mL of ether (Et2O) at 0° C. After stirring for 5 minutes, 5 mL of methanol was added. The reaction mixture was warmed to room temperature and kept there for 2.5 hours. Thereafter, 2.4 g more of lithium borohydride was added. The reaction mixture was quenched with aluminum chloride. After standard aqueous work up, and silica gel column purification (hexane/ethyl acetate 2:1), 4.0 g of 3-bromo-2-methoxy-phenyl-methanol 6 was obtained.
後処理
- waitkept there for 2.5 hours
- customThe reaction mixture was quenched with aluminum chloride
- customAfter standard aqueous work up, and silica gel column purification (hexane/ethyl acetate 2:1)
出典と根拠
- ORDレコード
- ord-f2de5ed57eaa450782d6e14a8cceec15
- 出典データセット
- uspto-grants-2015_05
- 特許番号
- US09034910B2
反応ノート
読み込み中…