Dimethylformamide → Anthranilic acid, N-dimethylaminomethylene-, methyl ester
反応式
[C:1]([O:10][CH3:11])(=[O:9])[C:2]1[C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[NH2:4].P(Cl)(Cl)(Cl)=O.[OH-].[Na+].[CH3:19][N:20]([CH3:23])[CH:21]=O>ClCCl>[CH3:19][N:20]([CH:23]=[N:4][C:3]1[CH:5]=[CH:6][CH:7]=[CH:8][C:2]=1[C:1]([O:10][CH3:11])=[O:9])[CH3:21]参加物
6
実験手順
To a stirred solution of 7.56 g of methyl anthranilate in 50 ml of dimethylformamide at 0° C. was added 5.6 ml of phosphorous oxychloride during 15 m. The mixture was heated at 55 for 45 m, cooled to 0, and diluted with dichloromethane. The mixture was basified at 0° C. by slow addition of cold 1N NaOH to pH 9. The dichloromethane layer was separated, washed with water, dried and concentrated to an oil.
後処理
- temperatureThe mixture was heated at 55 for 45 m
- temperaturecooled to 0
- customThe dichloromethane layer was separated
- washwashed with water
- customdried
- concentrationconcentrated to an oil
出典と根拠
- ORDレコード
- ord-4f854e02726a4bf3b5f84e05e395ec92
- 出典データセット
- uspto-grants-2002_05
- 特許番号
- US06384051B1
反応ノート
読み込み中…