Acetic Acid → HCID 73197187, 화합물

HRID 636725

반응식

HRID 636725 반응식
[CH3:1][C:2]([N+:5]([O-:7])=O)([CH3:4])[CH3:3].C(O)(=O)C.[N:12]1([C:17]2[CH:24]=[CH:23][C:20]([CH:21]=O)=[CH:19][CH:18]=2)[CH:16]=[CH:15][N:14]=[CH:13]1>C(O)C.[Zn]>[N:12]1([C:17]2[CH:24]=[CH:23][C:20]([CH:21]=[N+:5]([C:2]([CH3:4])([CH3:3])[CH3:1])[O-:7])=[CH:19][CH:18]=2)[CH:16]=[CH:15][N:14]=[CH:13]1

참가 물질

6

반응물 3

HCID 176Acetic AcidHCID 116722-Methyl-2-nitropropaneHCID 7365304-(1H-imidazol-1-yl)benzaldehyde

생성물 1

HCID 73197187HCID 73197187, 화합물

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 702Ethanol용매

반응 조건

온도
5 °C

실험 절차

To a suspension of 1,1-dimethylnitroethane (261.2 mg, 2.53 mmol) and zinc (247.0 mg, 3.78 mmol) in ethanol (3.0 ml) was added acetic acid (451.8 mg, 7.52 mmol) dropwise at 5° C. while stirring. The mixture was stirred at room temperature for 30 minutes. After cooling the mixture to 5° C. again, 4-(1-imidazolyl)benzaldehyde (216.5 mg, 1.26 mmol) was added dropwise to the mixture while stirring and stirred at room temperature overnight. Zinc acetate in the mixture was filtered off and the filtrate was concentrated and purified by silica gel chromatography (chloroform/methanol=10/1).

후처리

  1. stirringThe mixture was stirred at room temperature for 30 minutes
  2. stirringwhile stirring
  3. stirringstirred at room temperature overnight
  4. filtrationZinc acetate in the mixture was filtered off
  5. concentrationthe filtrate was concentrated
  6. custompurified by silica gel chromatography (chloroform/methanol=10/1)

출처 및 근거

ORD 기록
ord-bda5bfc6fee9495a97edd7e3f247ff2e
출처 데이터셋
uspto-grants-2001_02
특허 번호
US06194461B1

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