4,5-Dichloro-2-nitrobenzaldehyde → 2-Amino-4,5-dichlorobenzaldehyde

HRID 726642

반응식

HRID 726642 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C:7]([N+:11]([O-])=O)=[CH:8][C:9]=1[Cl:10])[CH:5]=[O:6]>C(O)C.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Fe+2]>[Cl:1][C:2]1[CH:3]=[C:4]([C:7]([NH2:11])=[CH:8][C:9]=1[Cl:10])[CH:5]=[O:6]

참가 물질

5

반응물 1

HCID 27492464,5-Dichloro-2-nitrobenzaldehyde

생성물 1

HCID 8180132-Amino-4,5-dichlorobenzaldehyde수율 86.8%

시약·촉매·용매 3

HCID 62662Ferrous sulfate heptahydrate촉매HCID 702Ethanol용매HCID 962Water용매

실험 절차

3,4-Dichloro-6-nitrobenzaldehyde (4.40 g, 20 mmol) was dissolved in 50% aqueous ethanol (200 ml) at 50°-60° C. and the solution was added to a solution of iron(II) sulfate heptahydrate (27.8 g, 100 mmol) in water (200 ml) at 90° C. Concentrated (25%) aqueous ammonia (50 ml) was added in several portions with intensive stirring while the temperature was kept close to the boiling point. The mixture was refluxed for 5-10 min. and cooled. The precipitate was filtered off and washed with ethanol. The filtrate was concentrated in vacuo until most of the ethanol was removed. The resulting precipitate was collected, washed with water and dried in vacuo at 40°-50° C. to give 3.3 g of 3,4-dichloro-6-aminobenzaldehyde.

후처리

  1. concentrationConcentrated (25%) aqueous ammonia (50 ml)
  2. additionwas added in several portions
  3. customwas kept close to the boiling point
  4. temperatureThe mixture was refluxed for 5-10 min.
  5. temperaturecooled
  6. filtrationThe precipitate was filtered off
  7. washwashed with ethanol
  8. concentrationThe filtrate was concentrated in vacuo until most of the ethanol
  9. customwas removed
  10. customThe resulting precipitate was collected
  11. washwashed with water
  12. customdried in vacuo at 40°-50° C.

출처 및 근거

ORD 기록
ord-2e39e3bdfd2e4393baa17f651f3c6417
출처 데이터셋
uspto-grants-1998_01
특허 번호
US05710139

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