HCID 23444980, 화합물 → 1-(3,4-dichloro-phenyl)-1H-imidazole-4-carbaldehyde

HRID 397895노트

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HRID 397895 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([N:9]2[CH:13]=[C:12]([CH2:14][OH:15])[N:11]=[CH:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8]>C1COCC1.O.[O-2].[Mn+4].[O-2]>[Cl:1][C:2]1[CH:3]=[C:4]([N:9]2[CH:13]=[C:12]([CH:14]=[O:15])[N:11]=[CH:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8]

참가 물질

5

반응물 1

HCID 23444980HCID 23444980, 화합물

생성물 1

HCID 234451021-(3,4-dichloro-phenyl)-1H-imidazole-4-carbaldehyde수율 25%

시약·촉매·용매 3

HCID 178418406HCID 178418406, 화합물촉매2회HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

A solution of [1-(3,4-dichloro-phenyl)-1H-imidazol-4-yl]-methanol (10.8 g, 44.3 mmol) in a mixture of THF (270 ml) and H2O (30 ml) was treated with manganese(IV) oxide (5 g, 57.5 mmol) and the mixture was refluxed for 4 h. A second portion of manganese(IV) oxide (1.5 g) was added and reflux continued for 1.5 h. The mixture was filtered over Celite, and the residue was washed with MeOH. Toluene was added to the filtrate, and the H2O was removed azeotropically. The brown residue was taken up in CH2Cl2 and upon standing white crystals formed. Filtration afforded 1-(3,4-dichloro-phenyl)-1H-imidazole-4-carbaldehyde (2.5 g, 25%). MS: m/e=240.0 (M+).

후처리

  1. temperaturethe mixture was refluxed for 4 h
  2. temperaturereflux
  3. filtrationThe mixture was filtered over Celite
  4. washthe residue was washed with MeOH
  5. additionToluene was added to the filtrate
  6. customthe H2O was removed azeotropically
  7. customformed
  8. filtrationFiltration

출처 및 근거

ORD 기록
ord-9f16cd0deed646e9a76af8dc9e30d03e
출처 데이터셋
uspto-grants-2003_08
특허 번호
US06610723B2

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