Potassium Carbonate → 3-(2,6-Dimethylbenzyloxy)-2-methoxybenzaldehyde
反応式
[OH:1][C:2]1[C:3]([O:10][CH3:11])=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH:5]=[O:6].[CH3:12][C:13]1[CH:20]=[CH:19][CH:18]=[C:17]([CH3:21])[C:14]=1[CH2:15]Cl.C([O-])([O-])=O.[K+].[K+]>CN(C=O)C.CCOC(C)=O>[CH3:12][C:13]1[CH:20]=[CH:19][CH:18]=[C:17]([CH3:21])[C:14]=1[CH2:15][O:1][C:2]1[C:3]([O:10][CH3:11])=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH:5]=[O:6]参加物
6
実験手順
The solution of 3-hydroxy-2-methoxybenzaldehyde (5.06 g, 32.7 mmol), 2,6-Dimethylbenzyl chloride (5.04 g, 33.1 mmol) and K2CO3 (4.78 g, 34.6 mmol) in dry DMF (15 ml) was stirred at room temperature under argon for 16 hours, then diluted with EtOAc (40 ml), and washed with water (20 ml). The organic layer was concentrated, and purified by flash chromatography on a silica gel column (hex: ethyl acetate 4:1) to give the title compound as an off white solid.
後処理
- washwashed with water (20 ml)
- concentrationThe organic layer was concentrated
- custompurified by flash chromatography on a silica gel column (hex: ethyl acetate 4:1)
出典と根拠
- ORDレコード
- ord-ac13b45dbc5043b08aa11032d69cd6ac
- 出典データセット
- uspto-grants-2014_11
- 特許番号
- US08889724B2
反応ノート
読み込み中…