N-benzyl-2-nitroaniline → N1-Benzylbenzene-1,2-diamine

HRID 1443622

Reaktionsgleichung

Reaktionsgleichung von HRID 1443622
[CH2:1]([NH:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[N+:15]([O-])=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>C(O)(=O)C.[Fe]>[CH2:1]([NH:8][C:9]1[C:10]([NH2:15])=[CH:11][CH:12]=[CH:13][CH:14]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

Komponenten

4

Edukt 1

HCID 521800N-benzyl-2-nitroaniline

Produkt 1

HCID 2735482N1-Benzylbenzene-1,2-diamine

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23925IronKatalysatorHCID 176Acetic AcidLösungsmittel

Reaktionsbedingungen

Temperatur
40 °C

Versuchsvorschrift

To a solution of Benzyl-(2-nitro-phenyl)-amine (230 mg, 1 mmol) in 3 ml acetic acid, was added iron (70 mg, 1.24 mmol). The reaction mixture was heated to 40° C. under argon for 2 hours. The mixture was cooled to ambient temperature and filtered through celite and the filtrate was concentrated. The resulting solid was dissolved in ethyl acetate. The organic layer was washed with saturated NaHCO3, dried over MgSO4, filtered and the filtrate was concentrated in vacuo to yield crude product that was used in step Example 5c.

Aufarbeitung

  1. temperatureThe mixture was cooled to ambient temperature
  2. filtrationfiltered through celite
  3. concentrationthe filtrate was concentrated
  4. dissolutionThe resulting solid was dissolved in ethyl acetate
  5. washThe organic layer was washed with saturated NaHCO3
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. concentrationthe filtrate was concentrated in vacuo
  9. customto yield crude product that

Quellen und Nachweise

ORD-Eintrag
ord-d0ed86af5dc04a5d9adfa9cb8722f05b
Quelldatensatz
uspto-grants-2010_02
Patentnummer
US07662581B1

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