Borane;tetrahydrofuran → (6-Amino-3-bromo-2-fluorophenyl)methanol
反応式
[NH2:1][C:2]1[C:7]([C:8](O)=[O:9])=[C:6]([F:11])[C:5]([Br:12])=[CH:4][CH:3]=1.B.C1COCC1>C1COCC1>[NH2:1][C:2]1[C:7]([CH2:8][OH:9])=[C:6]([F:11])[C:5]([Br:12])=[CH:4][CH:3]=1参加物
4
実験手順
To a solution of 6-amino-3-bromo-2-fluorobenzoic acid (9.0 g, 38.46 mmol) in THF (150 mL) was added BH3-THF (1 M, 193 mL) at 0° C., and the mixture was stirred at room temperature overnight. The reaction was slowly quenched with methanol (50 mL), and the solvents were removed under reduced pressure. The residue was diluted with 200 mL of ethyl acetate, washed with water (200 mL) and brine (200 mL), dried over sodium sulfate, filtered and concentrated to afford the title product (8.3 g, 98%), which was directly used in the next step without further purification. MS (ES+) C7H7BrFNO requires: 219, found: 220, 222 [M+H]+.
後処理
- customThe reaction was slowly quenched with methanol (50 mL)
- customthe solvents were removed under reduced pressure
- additionThe residue was diluted with 200 mL of ethyl acetate
- washwashed with water (200 mL) and brine (200 mL)
- dry with materialdried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-48efd38fab134ed9b2140e90274b5ab8
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09434700B2
反応ノート
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