Methanol → 2-Amino-6-bromophenol

HRID 469804

Reaktionsgleichung

Reaktionsgleichung von HRID 469804
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([Br:10])[C:5]=1[OH:11])([O-])=O.CO>C1COCC1.[Ni]>[NH2:1][C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([Br:10])[C:5]=1[OH:11]

Komponenten

5

Edukt 2

HCID 887MethanolHCID 135454532-Bromo-6-nitrophenol

Produkt 1

HCID 155315062-Amino-6-bromophenol

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 935NickelKatalysatorHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

5 g (22.9 mmol) 2-nitro-6-bromo-phenol (Fluka 67211) is hydrogenated in the presence of 0.1 g Ra—Ni (B113W EtOH, Degussa) in 100 ml of THF:MeOH=1:1. for 4 h. The reaction mixture is filtered (2 glass fiber filters used) and the filtrate is concentrated in vacuo. The residue is purified by chromatography (silicagel, hexane:EtOAc=2:1) to afford the title compound as a reddish oil which slowly solidifies.

Aufarbeitung

  1. filtrationThe reaction mixture is filtered (2 glass fiber filters used)
  2. concentrationthe filtrate is concentrated in vacuo
  3. customThe residue is purified by chromatography (silicagel, hexane:EtOAc=2:1)

Quellen und Nachweise

ORD-Eintrag
ord-991f4ad3cf6d4953aefaa3c986c6fd40
Quelldatensatz
uspto-grants-2014_01
Patentnummer
US08629168B2

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