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

HRID 1844598노트

반응식

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

2.0 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.

후처리

  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

출처 및 근거

ORD 기록
ord-30d8770e9e694482a6317da7ca4f6198
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08946438B2

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