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

HRID 379487

반응식

HRID 379487 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 (500 mL). Cool and extract ten times with diethyl ether. Dry the combined organic layers over Na2SO4, filter, and evaporate invacuo 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 invacuo
  7. customto give a residue

출처 및 근거

ORD 기록
ord-2f64c9662f21423cb61afebff02135b0
출처 데이터셋
uspto-grants-2001_10
특허 번호
US06297259B1

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