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

HRID 916081노트

반응식

HRID 916081 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 23994Zinc촉매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-d29a8f541a4647cdbb5b42e56acbe54f
출처 데이터셋
uspto-grants-2007_09
특허 번호
US07268145B2

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