反応式
[Br:1]N1C(=O)CCC1=O.[F:9][C:10]1[C:16]([C:17]([F:20])([F:19])[F:18])=[CH:15][CH:14]=[CH:13][C:11]=1[NH2:12].O>CN(C)C=O>[Br:1][C:15]1[CH:14]=[CH:13][C:11]([NH2:12])=[C:10]([F:9])[C:16]=1[C:17]([F:18])([F:19])[F:20]参加物
5
実験手順
A solution of N-bromosuccinimide (24.9 g) in N,N-dimethyl formamide was added to a solution of 2-fluoro-3-trifluoromethylaniline (25 g) in dimethyl formamide. The mixture was stirred for four and a half hours. It was poured into water and the oil was separated. The aqueous layers was extracted with ether and the combined organic layers were washed with water, dried (MgSO4) and filtered. The filtrate was evaporated to dryness and the residue was distilled to give 4-bromo-2-fluoro-3-trifluoromethylaniline (27.44 g) as an orange oil, b.p. 88°-94° C./4 mbar.
後処理
- customthe oil was separated
- extractionThe aqueous layers was extracted with ether
- washthe combined organic layers were washed with water
- dry with materialdried (MgSO4)
- filtrationfiltered
- customThe filtrate was evaporated to dryness
- distillationthe residue was distilled
出典と根拠
- ORDレコード
- ord-631dc0120bfa4282a8aa156e9f50f95d
- 出典データセット
- uspto-grants-1999_01
- 特許番号
- US05856274
関連ノート
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