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

HRID 1844598ノート

反応式

HRID 1844598 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]([CH:6]=1)[NH2:16])([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

2.0 g 5-tert-butyl-2-methoxy-1,3-dinitro-benzene are dissolved in 20 ml of ethanol, combined with 100 μl water and 100 mg of 10% palladium on activated charcoal and then refluxed. 1.9 ml of 4-methyl-cyclohexene are added and the mixture is refluxed for a further 2 hours. Then a further 950 μl of 4-methyl-cyclohexene are added dropwise and then refluxed for 16 hours. The solvents are then eliminated in vacuo, the residue is taken up in ethyl acetate and washed successively with saturated aqueous sodium hydrogen carbonate solution and saturated aqueous sodium chloride solution. After drying with sodium sulphate the solvents are eliminated in vacuo and the residue is dried in vacuo.

後処理

  1. temperaturerefluxed
  2. temperaturethe mixture is refluxed for a further 2 hours
  3. temperaturerefluxed for 16 hours
  4. washwashed successively with saturated aqueous sodium hydrogen carbonate solution and saturated aqueous sodium chloride solution
  5. dry with materialAfter drying with sodium sulphate the solvents
  6. customthe residue is dried in vacuo

出典と根拠

ORDレコード
ord-30d8770e9e694482a6317da7ca4f6198
出典データセット
uspto-grants-2015_02
特許番号
US08946438B2

反応ノート

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