Water → 5-(tert-Butyl)-2-methoxy-3-nitroaniline

HRID 2360512노트

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HRID 2360512 반응식
[C:1]([C:5]1[CH:6]=[C:7]([N+:16]([O-])=O)[C:8]([O:14][CH3:15])=[C:9]([N+:11]([O-:13])=[O:12])[CH:10]=1)([CH3:4])([CH3:3])[CH3:2].O.CC1CCC=CC1>C(O)C.[Pd].C(OCC)(=O)C>[C:1]([C:5]1[CH:10]=[C:9]([N+:11]([O-:13])=[O:12])[C:8]([O:14][CH3:15])=[C:7]([NH2:16])[CH:6]=1)([CH3:4])([CH3:2])[CH3:3]

참가 물질

7

반응물 3

HCID 962WaterHCID 115724-Methylcyclohexene2회HCID 42526024-tert-Butyl-2,6-dinitroanisole

생성물 1

HCID 112068635-(tert-Butyl)-2-methoxy-3-nitroaniline

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 702Ethanol용매HCID 8857Ethyl Acetate용매

실험 절차

2 g 5-tert-butyl-2-methoxy-1,3-dinitro-benzene are dissolved in 20 ml ethanol and combined with 2 ml of water and 100 mg of 10% palladium on charcoal. The mixture is refluxed, 1.9 ml of 4-methyl-1-cyclohexene are added and the mixture is refluxed for a further 2 hours. Then a further 1.0 ml of 4-methyl-1-cyclohexene are added dropwise and the mixture is refluxed for a further 16 hours. Then it is cooled to ambient temperature, the solvents are eliminated in vacuo and the residue is taken up in ethyl acetate. The mixture is washed with saturated aqueous sodium hydrogen carbonate solution, water, saturated aqueous sodium chloride solution and dried with sodium sulphate. The solvent is eliminated in vacuo and the product thus obtained is further reacted directly.

후처리

  1. temperatureThe mixture is refluxed
  2. temperaturethe mixture is refluxed for a further 2 hours
  3. temperaturethe mixture is refluxed for a further 16 hours
  4. washThe mixture is washed with saturated aqueous sodium hydrogen carbonate solution, water, saturated aqueous sodium chloride solution
  5. dry with materialdried with sodium sulphate
  6. customthe product thus obtained
  7. customis further reacted directly

출처 및 근거

ORD 기록
ord-6834b957faa846118be0c825c6794cb0
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08686022B2

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