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1,2,4,5-Tetrafluoro-3-methoxy-6-nitrobenzene → 4-Methoxy-2-phthalimido-3,5,6-trifluoro-1-nitrobenzene

HRID 358868
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HRID 358868 반응식
[C:1]1(=[O:11])[NH:5][C:4](=[O:6])[C:3]2=[CH:7][CH:8]=[CH:9][CH:10]=[C:2]12.[K].[CH3:13][O:14][C:15]1[C:20]([F:21])=[C:19](F)[C:18]([N+:23]([O-:25])=[O:24])=[C:17]([F:26])[C:16]=1[F:27]>CN(C)C=O>[CH3:13][O:14][C:15]1[C:16]([F:27])=[C:17]([F:26])[C:18]([N+:23]([O-:25])=[O:24])=[C:19]([N:5]2[C:1](=[O:11])[C:2]3=[CH:10][CH:9]=[CH:8][CH:7]=[C:3]3[C:4]2=[O:6])[C:20]=1[F:21]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 42613721,2,4,5-Tetrafluoro-3-methoxy-6-nitrobenzeneHCID 24194345Phthalimide potassium salt

생성물 1

HCID 200671344-Methoxy-2-phthalimido-3,5,6-trifluoro-1-nitrobenzene수율 60%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

4.62 g (0.025 mole) of potassium phthalimide were added to a solution of 5.41 g (0.024 mole) of 4-methoxy-2,3,5,6-tetrafluoro-1-nitrobenzene (XXXIII) in 100 ml of dimethylformamide, and the mixture was stirred at room temperature for 3 hours. At the end of this time, the solvent was removed by evaporation under reduced pressure, the residue was dissolved in toluene, and the solution was washed with water, dried and concentrated by evaporation under reduced pressure to give an oily substance. This oily substance was subjected to silica gel column chromatography eluted with toluene, to afford 5.07 g of 4-methoxy-2-phthalimido-3,5,6-trifluoro-1-nitrobenzene (XXXIV) as pale yellow powdery crystals.

후처리

  1. customAt the end of this time, the solvent was removed by evaporation under reduced pressure
  2. dissolutionthe residue was dissolved in toluene
  3. washthe solution was washed with water
  4. customdried
  5. concentrationconcentrated by evaporation under reduced pressure
  6. customto give an oily substance
  7. washeluted with toluene

출처 및 근거

ORD 기록
ord-aadd31a63e784190b9647379efa783e7
출처 데이터셋
uspto-grants-1991_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04997943

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