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Hexamethylenetetramine → 4-Methoxy-3-(trifluoromethyl)benzaldehyde

HRID 2300130
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HRID 2300130 반응식
[F:1][C:2]([F:12])([F:11])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[O:9][CH3:10].C1N2CN3CN(C2)CN1C3.FC(F)(F)[C:25](O)=[O:26]>>[F:1][C:2]([F:11])([F:12])[C:3]1[CH:8]=[C:7]([CH:6]=[CH:5][C:4]=1[O:9][CH3:10])[CH:25]=[O:26]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 4101HexamethylenetetramineHCID 6422Trifluoroacetic acidHCID 27752511-Methoxy-2-(trifluoromethyl)benzene

생성물 1

HCID 27752914-Methoxy-3-(trifluoromethyl)benzaldehyde

실험 절차

A mixture of 8.5 g 2-trifluoromethyl anisole and 7.0 g hexamethylene tetramine was stirred at 90° C. for 1.5 hr in 80 ml trifluoroacetic acid. The reaction solution was evaporated. The resulting residue was dissolved in ethyl acetate, and it was added dropwise into ice-cooled saturated aqueous sodium bicarbonate. The ethyl acetate layer was recovered and washed with brine. It was dried over anhydrous magnesium sulfate, filtered, and evaporated. The resulting residue was purified by silica gel column chromatography to give 5.8 g of 3-trifluoromethyl-p-anisaldehyde.

후처리

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트
  • customThe reaction solution was evaporated
  • dissolutionThe resulting residue was dissolved in ethyl acetate
  • additionit was added dropwise into ice-
  • temperaturecooled saturated aqueous sodium bicarbonate
  • customThe ethyl acetate layer was recovered
  • washwashed with brine
  • dry with materialIt was dried over anhydrous magnesium sulfate
  • filtrationfiltered
  • customevaporated
  • customThe resulting residue was purified by silica gel column chromatography
  • 출처 및 근거

    ORD 기록
    ord-ed346788d6fc41e588430e09a75b3d6a
    출처 데이터셋
    uspto-grants-2002_12
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US06498159B1

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