Water → Benzoic acid, 3-methoxy-2-nitro-, methyl ester
反応式
[CH3:1][O:2][C:3]1[C:4]([N+:12]([O-:14])=[O:13])=[C:5]([CH:9]=[CH:10][CH:11]=1)[C:6]([OH:8])=[O:7].[C:15]([O-])([O-])=O.[K+].[K+].CI.O>CN(C=O)C>[CH3:1][O:2][C:3]1[C:4]([N+:12]([O-:14])=[O:13])=[C:5]([CH:9]=[CH:10][CH:11]=1)[C:6]([O:8][CH3:15])=[O:7]参加物
6
実験手順
To a mixture of 3-methoxy-2-nitrobenzoic acid (25.0 g, 126 mmol) and K2CO3 (35.0 g, 253 mmol) in DMF (126 mL) was added MeI (15.8 mL, 253 mmol) at room temperature. The mixture was stirred at room temperature for 2 hours. To the mixture was poured the water (200 mL) and then stirred at 5° C. for 30 min. The precipitated solid was collected by filtration, washed with water and hexane. The solid was dried under reduced pressure to afford the compound 52 in a crude form (26.2 g, 98%) as a white solid.
後処理
- stirringstirred at 5° C. for 30 min
- filtrationThe precipitated solid was collected by filtration
- washwashed with water and hexane
- customThe solid was dried under reduced pressure
出典と根拠
- ORDレコード
- ord-fb38c9e1c3204998875316fa067af5e4
- 出典データセット
- uspto-grants-2015_05
- 特許番号
- US09034921B2
反応ノート
読み込み中…