Diethyl Ether → 4-Bromo-2-fluoro-5-(methoxymethoxy)benzaldehyde
反応式
[Br:1][C:2]1[C:9]([OH:10])=[CH:8][C:5]([CH:6]=[O:7])=[C:4]([F:11])[CH:3]=1.[CH2:12](Cl)[O:13][CH3:14].[H-].[Na+].CCOCC>CN(C)C=O>[Br:1][C:2]1[C:9]([O:10][CH2:12][O:13][CH3:14])=[CH:8][C:5]([CH:6]=[O:7])=[C:4]([F:11])[CH:3]=1参加物
6
反応条件
- 温度
- 0 °C
実験手順
4-Bromo-2-fluoro-5-hydroxy-benzaldehyde (750 mg, 3.41 mmol) and MOMCl (545 mg, 6.82 mmol) were dissolved in anhydrous N,N-dimethylformamide (5 mL) and cooled to 0° C. NaH (160 mg, 60% suspension in mineral oil, 4 mmol) is then added. The resulting mixture is allowed to stir at room temperature for 1 h. Ether is then added and washed with H2O (3×20 mL) and brine. After dried over Na2SO4, the ether is removed and the residue is purified through chromatography to afford the desired MOM ether (700 mg, 78%).
後処理
- washwashed with H2O (3×20 mL) and brine
- dry with materialAfter dried over Na2SO4
- customthe ether is removed
- customthe residue is purified through chromatography
- customto afford the desired MOM ether (700 mg, 78%)
出典と根拠
- ORDレコード
- ord-e1922472764e430ba5b08652c2d7bf12
- 出典データセット
- uspto-grants-2010_05
- 特許番号
- US07713994B2
反応ノート
読み込み中…