反応式
F[C:2]1[CH:3]=[C:4]([O:11][C:12]2[CH:17]=[C:16]([F:18])[C:15]([C:19]([F:22])([F:21])[F:20])=[C:14]([Cl:23])[CH:13]=2)[CH:5]=[CH:6][C:7]=1[N+:8]([O-:10])=[O:9].[NH2:24][C:25]1[CH:36]=[CH:35][C:28]([O:29][CH2:30][C:31]([O:33][CH3:34])=[O:32])=[CH:27][CH:26]=1.C(=O)([O-])[O-].[K+].[K+].C(OCC)(=O)C>CN(C)C=O.[Cl-].[Na+].O>[Cl:23][C:14]1[CH:13]=[C:12]([O:11][C:4]2[CH:5]=[CH:6][C:7]([N+:8]([O-:10])=[O:9])=[C:2]([CH:3]=2)[NH:24][C:25]2[CH:26]=[CH:27][C:28]([O:29][CH2:30][C:31]([O:33][CH3:34])=[O:32])=[CH:35][CH:36]=2)[CH:17]=[C:16]([F:18])[C:15]=1[C:19]([F:20])([F:22])[F:21]参加物
7
反応物 4
生成物 1
試薬・触媒・溶媒 2
反応条件
- 温度
- 80 °C
実験手順
A mixture of 2-chloro-α,α,α,6-tetrafluoro-p-tolyl 3-fluoro-4-nitrophenyl ether (2.1 g, 0.006 mol), methyl (p-aminophenoxy)acetate (2.7 g, 0.015 mol) and potassium carbonate (2.0 g, 0,015 mol) in N,N-dimethyl formamide is stirred at 80° C. for 18 hours, cooled to room temperature, poured into brine and extracted with ethyl acetate. The organic extract is washed with brine, dried over anhydrous sodium sulfate and concentrated in vacuo to obtain a residue. Flash chromatography of the residue using silica gel and a 20% ethyl acetate in hexanes solution gives the title product as a red oil (0.6 g) which is identified by 1HNMR and 13CNMR spectral analyses.
後処理
- temperaturecooled to room temperature
- extractionextracted with ethyl acetate
- extractionThe organic extract
- washis washed with brine
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated in vacuo
- customto obtain a residue
出典と根拠
- ORDレコード
- ord-83e80843e5f64dcf9c75d52225a97513
- 出典データセット
- uspto-grants-1995_06
- 特許番号
- US05424280
関連ノート
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