Chlorosuccinimide → 4-Chloro-2,3-difluoro-6-nitroaniline
反応式
[F:1][C:2]1[C:8]([F:9])=[CH:7][CH:6]=[C:5]([N+:10]([O-:12])=[O:11])[C:3]=1[NH2:4].[Cl:13]N1C(=O)CCC1=O>CN(C)C=O>[Cl:13][C:7]1[CH:6]=[C:5]([N+:10]([O-:12])=[O:11])[C:3]([NH2:4])=[C:2]([F:1])[C:8]=1[F:9]参加物
4
反応条件
- 温度
- 85 °C
実験手順
2,3-Difluoro-6-nitroaniline (15.4 g, 88.7 mmol), N-chlorosuccinimide (14.9 g, 111.4 mmol) and N,N-dimethylformamide (250 mL) were combined and were heated to 80-90° C. for several hours, after which time the mixture was poured into ice water. The product was extracted with ethyl acetate which was then washed with water, saturated aqueous sodium chloride, dried over magnesium sulfate, filtered and the solvents were removed in vacuo to leave a yellow, viscous oil. 1H NMR (DMSO-d6) δ: 8.03 (dd, J=7.3, 2.2 Hz, 1H, Ar—H), 7.65 (br s, 2H, NH2).
後処理
- extractionThe product was extracted with ethyl acetate which
- washwas then washed with water, saturated aqueous sodium chloride
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- customthe solvents were removed in vacuo
- customto leave a yellow, viscous oil
出典と根拠
- ORDレコード
- ord-482413f54be44b608a4a9dfcb7b81063
- 出典データセット
- uspto-grants-2002_07
- 特許番号
- US06413938B1
反応ノート
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