Chlorosuccinimide → 2,3,4-Trichloro-6-nitrobenzenamine
反応式
[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][C:5]([NH2:9])=[C:4]([N+:10]([O-:12])=[O:11])[CH:3]=1.[Cl:13]N1C(=O)CCC1=O>CN(C=O)C>[Cl:13][C:6]1[C:7]([Cl:8])=[C:2]([Cl:1])[CH:3]=[C:4]([N+:10]([O-:12])=[O:11])[C:5]=1[NH2:9]参加物
4
反応条件
- 温度
- 100 °C
実験手順
A mixture of 4,5-dichloro-2-nitro-phenylamine (0.500 g, 2.42 mmol), N-chlorosuccinimide (0.403 g, 3.02 mmol), and DMF (5 mL) was heated to 100° C. for 1 h. After cooling to 23° C., the solution was poured into ice water. The yellow precipitate was collected by filtration and dissolved in dichloromethane. The organic phase was washed with water, dried (MgSO4), filtered, and concentrated to yield the titled compound (0.468 g, 81%). 1H NMR (400 MHz, CDCl3): 8.28 (s, 1H), 6.70 (s, 2H). The compound did not yield MS data.
後処理
- temperatureAfter cooling to 23° C.
- filtrationThe yellow precipitate was collected by filtration
- dissolutiondissolved in dichloromethane
- washThe organic phase was washed with water
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-da960d27c9fb455294a994e374f10859
- 出典データセット
- uspto-grants-2014_06
- 特許番号
- US08759345B2
反応ノート
読み込み中…