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

HRID 1743395

反応式

HRID 1743395 の反応式
[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]

参加物

5

反応物 2

HCID 5964652,3-Dimethyl-4-nitroanisoleHCID 178418361HCID 178418361、化合物

生成物 1

HCID 110948094-Methoxy-2,3-dimethylaniline収率 70%

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-41a00319aad84bef96212bf30c6ab15a
出典データセット
uspto-grants-2006_03
特許番号
US07008940B1

関連ノート

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