(E)-Methyl 2-(2-(dimethylamino)vinyl)-3-nitrobenzoate → 5-nitro-1H-isochromen-1-one
反応式
CN(C)/C=[CH:4]/[C:5]1[C:14]([N+:15]([O-:17])=[O:16])=[CH:13][CH:12]=[CH:11][C:6]=1[C:7]([O:9][CH3:10])=[O:8]>CCOC(C)=O>[N+:15]([C:14]1[CH:13]=[CH:12][CH:11]=[C:6]2[C:5]=1[CH:4]=[CH:10][O:9][C:7]2=[O:8])([O-:17])=[O:16]参加物
3
実験手順
(E)-Methyl 2-(2-(dimethylamino)vinyl)-3-nitrobenzoate was dissolved in EtOAc (200 mL), and silica gel (200 g) was added. The resulting suspension was stirred at room temperature for 1 h. The EtOAc solution was filtered off. Silica gel was washed with EtOAc (2×150 mL) and the combined organics were evaporated and dried under reduced pressure to yield 5-nitro-1H-isochromen-1-one (4.0 g, 21.0 mmol, 82% after two steps) of as a brown solid.
後処理
- additionsilica gel (200 g) was added
- filtrationThe EtOAc solution was filtered off
- washSilica gel was washed with EtOAc (2×150 mL)
- customthe combined organics were evaporated
- customdried under reduced pressure
出典と根拠
- ORDレコード
- ord-cf36175bb37347578b6f3ee99fd73590
- 出典データセット
- uspto-grants-2010_10
- 特許番号
- US07816371B2
反応ノート
読み込み中…