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

HRID 564295노트

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HRID 564295 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

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온도
50 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-746c4d7cf3d848e2befd053d5d04fc02
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08067638B2

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