Hydrochloric Acid → 2-Methoxy-5-(trifluoromethyl)aniline

HRID 868399

반응식

HRID 868399 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]([F:12])([F:11])[F:10])=[CH:5][C:4]=1[N+:13]([O-])=O.Cl>C(O)(C)C.O.[Fe]>[NH2:13][C:4]1[CH:5]=[C:6]([C:9]([F:10])([F:11])[F:12])[CH:7]=[CH:8][C:3]=1[O:2][CH3:1]

참가 물질

6

반응물 2

HCID 313Hydrochloric AcidHCID 967482-Nitro-4-trifluoromethylanisole

생성물 1

HCID 6006372-Methoxy-5-(trifluoromethyl)aniline수율 82.8%

시약·촉매·용매 3

HCID 23925Iron촉매HCID 962Water용매HCID 3776Isopropanol용매

반응 조건

온도
50 °C

실험 절차

4-Methoxy-3-nitrobenzotrifluoride (95 g) in isopropanol (1.0 liter) and water (250 ml) was mixed with concentrated hydrochloric acid (15 ml). Iron powder (180 g) was added and the mixture was heated and stirred under reflux. After 90 minutes the mixture was cooled to 50° C. and filtered. The residue was washed with isopropanol and the combined filtrates evaporated. The residue was dissolved in toluene and the solution dried (MgSO4) and evaporated. The residue was triturated with light petroleum (b.p. 30°-40°) to give the 3-amino-4-methoxybenzotrifluoride as a colourless solid (68 g).

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux
  3. filtrationfiltered
  4. washThe residue was washed with isopropanol
  5. customthe combined filtrates evaporated
  6. dissolutionThe residue was dissolved in toluene
  7. dry with materialthe solution dried (MgSO4)
  8. customevaporated
  9. customThe residue was triturated with light petroleum (b.p. 30°-40°)

출처 및 근거

ORD 기록
ord-5eb17cae1abe4f1f8240e585bdc7150e
출처 데이터셋
uspto-grants-1988_10
특허 번호
US04778914

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