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

HRID 2360512ノート

反応式

HRID 2360512 の反応式
[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]

参加物

7

反応物 3

HCID 962WaterHCID 115724-Methylcyclohexene2 回HCID 42526024-tert-Butyl-2,6-dinitroanisole

生成物 1

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

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 702Ethanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6834b957faa846118be0c825c6794cb0
出典データセット
uspto-grants-2014_04
特許番号
US08686022B2

反応ノート

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