Water → 4-[(2-Chloro-alpha,alpha,alpha,6-tetrafluoro-p-tolyl)oxy]-2-(p-methoxyphenoxy)-1-nitrobenzene

HRID 21510

반응식

HRID 21510 반응식
[N+]([C:4]1[CH:5]=[C:6]([O:13][C:14]2[CH:19]=[C:18]([F:20])[C:17]([C:21]([F:24])([F:23])[F:22])=[C:16]([Cl:25])[CH:15]=2)[CH:7]=[CH:8][C:9]=1[N+:10]([O-:12])=[O:11])([O-])=O.[CH3:26][O:27][C:28]1[CH:33]=[CH:32][C:31]([OH:34])=[CH:30][CH:29]=1.C(=O)([O-])[O-].[K+].[K+].O>C(#N)C>[Cl:25][C:16]1[CH:15]=[C:14]([O:13][C:6]2[CH:7]=[CH:8][C:9]([N+:10]([O-:12])=[O:11])=[C:4]([O:34][C:31]3[CH:32]=[CH:33][C:28]([O:27][CH3:26])=[CH:29][CH:30]=3)[CH:5]=2)[CH:19]=[C:18]([F:20])[C:17]=1[C:21]([F:22])([F:24])[F:23]

참가 물질

6

반응물 4

HCID 962WaterHCID 90154-MethoxyphenolHCID 11430Potassium CarbonateHCID 867487112-Chloro-alpha,alpha,alpha,6-tetrafluoro-p-tolyl 3,4-dinitrophenyl ether

생성물 1

HCID 867487124-[(2-Chloro-alpha,alpha,alpha,6-tetrafluoro-p-tolyl)oxy]-2-(p-methoxyphenoxy)-1-nitrobenzene수율 25.2%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A mixture of 2-chloro-α,α,α,6-tetrafluoro-p-tolyl 3,4-dinitrophenyl ether (10.0 g, 0.026 mol), 4methoxyphenol (6.45 g, 0.052 mol) and potassium carbonate (7.26 g, 0.052 mol) in acetonitrile is refluxed for 18 hours, cooled to room temperature, poured into water and extracted with ethyl acetate. The organic extract is washed with brine, dried over anhydrous sodium sulfate and concentrated in vacuo to obtain an amber oil. Column chromatography of the oil using silica gel and a (1:4) ether/hexanes solution gives the title product as a yellow oil (3.0 g) which is identified by 1HNMR and 13CNMR spectral analyses.

후처리

  1. temperatureis refluxed for 18 hours
  2. extractionextracted with ethyl acetate
  3. extractionThe organic extract
  4. washis washed with brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated in vacuo
  7. customto obtain an amber oil

출처 및 근거

ORD 기록
ord-e3ab984d5c024708ae7185b42301c498
출처 데이터셋
uspto-grants-1995_06
특허 번호
US05424280

연결된 노트

불러오는 중…