Ethanol → ((1-Naphthyl)methyl)(2-amino-4-methyl-phenyl)amine

HRID 916081ノート

反応式

HRID 916081 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([NH2:8])=[C:4]([N+:9]([O-])=O)[CH:3]=1.[CH2:12](O)[CH3:13].[OH-].[Na+].O1[CH2:22][CH2:21]OCC1>[Zn]>[C:12]1([CH2:13][NH:8][C:5]2[CH:6]=[CH:7][C:2]([CH3:1])=[CH:3][C:4]=2[NH2:9])[C:21]2[C:22](=[CH:1][CH:2]=[CH:3][CH:4]=2)[CH:7]=[CH:6][CH:5]=1

参加物

6

反応物 4

HCID 702EthanolHCID 69784-Methyl-2-nitroanilineHCID 14798Sodium HydroxideHCID 312751,4-Dioxane

生成物 1

HCID 17810729((1-Naphthyl)methyl)(2-amino-4-methyl-phenyl)amine

試薬・触媒・溶媒 1

HCID 23994Zinc触媒

実験手順

To (1-naphthyl)methyl)(4-methyl-2-nitro-phenyl)amine (1.0021 g, 3.43 mmol), ethanol (5 ml) and 1,4-dioxane (5 ml) were added, and 2.058 M aqueous sodium hydroxide solution (1 ml) was further added, and refluxed in an oil bath. After 15 minutes, it was removed from the oil bath, and zinc powder (897 mg, 13.72 mmol) was fed thereto in portions. Then it was refluxed again in the oil bath for 2 hours. After 2 hours, it was concentrated under reduced pressure, and dissolved in ethyl acetate (50 ml), and washed twice with saturated saline (25 ml). After drying with magnesium sulfate, it was concentrated under reduced pressure and dried to obtain a brown oil of ((1-naphthyl)methyl)(2-amino-4-methyl-phenyl)amine (943.1 mg).

後処理

  1. temperaturerefluxed in an oil bath
  2. temperatureThen it was refluxed again in the oil bath for 2 hours
  3. waitAfter 2 hours
  4. concentrationit was concentrated under reduced pressure
  5. dissolutiondissolved in ethyl acetate (50 ml)
  6. washwashed twice with saturated saline (25 ml)
  7. dry with materialAfter drying with magnesium sulfate, it
  8. concentrationwas concentrated under reduced pressure
  9. customdried

出典と根拠

ORDレコード
ord-d29a8f541a4647cdbb5b42e56acbe54f
出典データセット
uspto-grants-2007_09
特許番号
US07268145B2

反応ノート

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