Sulfuric Acid → 2-Methoxy-5-(trifluoromethoxy)benzaldehyde

HRID 582083

반응식

HRID 582083 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([O:9][C:10]([F:13])([F:12])[F:11])=[CH:5][CH:4]=1.FC(F)(F)[C:16](O)=[O:17].C1N2CN3CN(C2)CN1C3.S(=O)(=O)(O)O>C(OCC)(=O)C.CCCCCC>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([O:9][C:10]([F:11])([F:12])[F:13])=[CH:5][C:4]=1[CH:16]=[O:17]

참가 물질

6

반응물 4

HCID 1118Sulfuric AcidHCID 4101HexamethylenetetramineHCID 6422Trifluoroacetic acidHCID 27249731-Methoxy-4-(trifluoromethoxy)benzene

생성물 1

HCID 27833642-Methoxy-5-(trifluoromethoxy)benzaldehyde

시약·촉매·용매 1

HCID 21226206Ethyl acetate hexane용매

반응 조건

온도
60 °C

실험 절차

Combine 2-methoxy-5-trifluoromethoxybenzene (1.0 g, 5.2 mmol) and trifluoroacetic acid (200 mL). Add slowly portionwise hexamethylenetetraamine (26 g, 185.7 mmol). Heat at 60° C. After 24 hours, cool to ambient temperature and pour the reaction mixture into a 2M aqueous solution of sulfuric acid (500mL). Cool and extract ten times with diethyl ether. Dry the combined organic layers over Na2SO4, filter, and evaporate in vacuo to give a residue. Chromatograph the residue on silica gel eluting with 1/4 ethyl acetate/hexane to give 2-methoxy-5-trifluoromethoxybenzaldehyde.

후처리

  1. temperaturecool to ambient temperature
  2. temperatureCool
  3. extractionextract ten times with diethyl ether
  4. dry with materialDry the combined organic layers over Na2SO4
  5. filtrationfilter
  6. customevaporate in vacuo
  7. customto give a residue

출처 및 근거

ORD 기록
ord-c70067c0f9174d6a9b46f889f89f743a
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05922737

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