4-Nitrophenol → 1-(1,1,2,3,3,3-Hexafluoropropoxy)-4-nitrobenzene

HRID 564295ノート

反応式

HRID 564295 の反応式
[CH:1]1[C:6]([N+:7]([O-:9])=[O:8])=[CH:5][CH:4]=[C:3]([OH:10])[CH:2]=1.O.[K].CN(C)C=O.[F:18][C:19]([F:26])([F:25])[C:20]([F:24])=[C:21]([F:23])[F:22]>O.C(OCC)(=O)C>[F:22][C:21]([F:23])([O:10][C:3]1[CH:4]=[CH:5][C:6]([N+:7]([O-:9])=[O:8])=[CH:1][CH:2]=1)[CH:20]([F:24])[C:19]([F:26])([F:25])[F:18]

参加物

7

反応物 4

HCID 9804-NitrophenolHCID 6228DimethylformamideHCID 8302HexafluoropropyleneHCID 5347118072414-64-3

生成物 1

HCID 713656861-(1,1,2,3,3,3-Hexafluoropropoxy)-4-nitrobenzene収率 42%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
50 °C

実験手順

To a solution of 4.63 g of p-nitrophenol and 0.56 g of potassium hydrate added to 100 ml of N,N-dimethylformamide blowed hexafluoropropene at room temperature, and then the solution was stirred at 50° C. for 1 hour. Next, ethyl acetate and water were introduced in the reaction solution for separating the organic phase. The organic phase was dried over anhydrous sodium sulfate and the solvent was removed under a reduced pressure. The resulting residue was purified by silica gel column chromatography (n-hexane:EtOAc=20:1) to obtain 3.81 g of the desired product (Yield: 42%) as a yellow oil.

後処理

  1. customat room temperature
  2. customfor separating the organic phase
  3. dry with materialThe organic phase was dried over anhydrous sodium sulfate
  4. customthe solvent was removed under a reduced pressure
  5. customThe resulting residue was purified by silica gel column chromatography (n-hexane:EtOAc=20:1)

出典と根拠

ORDレコード
ord-746c4d7cf3d848e2befd053d5d04fc02
出典データセット
uspto-grants-2011_11
特許番号
US08067638B2

反応ノート

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