Water → 1-Fluoro-4-(4-nitrophenoxy)-2-(trifluoromethyl)benzene

HRID 17671

反応式

HRID 17671 の反応式
F[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][CH:3]=1.[F:11][C:12]1[CH:17]=[CH:16][C:15]([OH:18])=[CH:14][C:13]=1[C:19]([F:22])([F:21])[F:20].C(=O)([O-])[O-].[K+].[K+].O>CN(C=O)C>[F:11][C:12]1[CH:17]=[CH:16][C:15]([O:18][C:2]2[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][CH:3]=2)=[CH:14][C:13]=1[C:19]([F:20])([F:21])[F:22]

参加物

6

反応物 4

HCID 962WaterHCID 9590p-FluoronitrobenzeneHCID 11430Potassium CarbonateHCID 6018544-Fluoro-3-(trifluoromethyl)phenol

生成物 1

HCID 669776401-Fluoro-4-(4-nitrophenoxy)-2-(trifluoromethyl)benzene

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
90 °C

実験手順

To a stirred solution of 4-fluoronitrobenzene (20 mmol), 4-fluoro-3-trifluoromethylphenol (22 mmol) in DMF (50 mL) at rt, solid potassium carbonate (60 mmol) was added, and the reaction mixture was heated to 90° C. for 5 h (monitored by TLC), according to General Procedure L1. After cooling to rt, the reaction mixture was poured into cold H2O (60 mL). The resulting mixture was extracted with EtOAc (3×100 mL). The combined EtOAc extracts were washed with H2O (2×40 mL) and brine (50 mL), and dried over anhydrous sodium sulfate. The solvent was removed in vacuuo to afford the desired 1-fluoro-4-(4-nitrophenoxy)-2-(trifluoromethyl)benzene. The crude product was used directly for further transformation without further purification.

後処理

  1. temperatureAfter cooling to rt
  2. extractionThe resulting mixture was extracted with EtOAc (3×100 mL)
  3. washThe combined EtOAc extracts were washed with H2O (2×40 mL) and brine (50 mL)
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe solvent was removed in vacuuo

出典と根拠

ORDレコード
ord-b643970d821c41aea9833f961ae9e5b7
出典データセット
uspto-grants-2010_06
特許番号
US07737285B2

関連ノート

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