2,3-Dimethyl-4-nitroanisole → 4-Methoxy-2,3-dimethylaniline

HRID 1743395

반응식

HRID 1743395 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([N+:9]([O-])=O)=[C:5]([CH3:12])[C:4]=1[CH3:13].[H][H]>C(O)C.[C].[Pd]>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([NH2:9])=[C:5]([CH3:12])[C:4]=1[CH3:13]

참가 물질

5

반응물 2

HCID 5964652,3-Dimethyl-4-nitroanisoleHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 110948094-Methoxy-2,3-dimethylaniline수율 70%

시약·촉매·용매 2

HCID 178418390HCID 178418390, 화합물촉매HCID 702Ethanol용매

실험 절차

4-Methoxy-2,3-dimethylnitrobenzene (21.1 g, 0.15 mol) was dissolved in ethanol (300 mL), and 10% palladium carbon (50% hydrate, 1.36 g) was added. The mixture was reacted at 40° C. for 2 hours under the hydrogen atmosphere. After cooling, the catalyst was removed, ethanol was distilled off under reduced pressure, and the residue was diluted with ethyl acetate. The dilution was washed with 5% sodium hydrosulfite, dried over sodium sulfate, and purified by small amount silica gel column chromatography (ethyl acetate, 1:1). The solvent was distilled off under reduced pressure, followed by recrystallization from hexane, to obtain 15.8 g of the title compound.

후처리

  1. temperatureAfter cooling
  2. customthe catalyst was removed
  3. distillationethanol was distilled off under reduced pressure
  4. additionthe residue was diluted with ethyl acetate
  5. washThe dilution was washed with 5% sodium hydrosulfite
  6. dry with materialdried over sodium sulfate
  7. custompurified by small amount silica gel column chromatography (ethyl acetate, 1:1)
  8. distillationThe solvent was distilled off under reduced pressure
  9. customfollowed by recrystallization from hexane

출처 및 근거

ORD 기록
ord-41a00319aad84bef96212bf30c6ab15a
출처 데이터셋
uspto-grants-2006_03
특허 번호
US07008940B1

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