Chlorosuccinimide → 2,3,4-Trichloro-6-nitrobenzenamine
반응식
[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]참가 물질
4
반응 조건
- 온도
- 100 °C
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-da960d27c9fb455294a994e374f10859
- 출처 데이터셋
- uspto-grants-2014_06
- 특허 번호
- US08759345B2
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