Iodine → Methyl 4-amino-3-iodo-5-nitrobenzoate

HRID 59804

Reaktionsgleichung

Reaktionsgleichung von HRID 59804
[CH3:1][O:2][C:3](=[O:14])[C:4]1[CH:9]=[CH:8][C:7]([NH2:10])=[C:6]([N+:11]([O-:13])=[O:12])[CH:5]=1.[I:15]I>C(O)C.[O-]S([O-])(=O)=O.[Ag+].[Ag+]>[CH3:1][O:2][C:3](=[O:14])[C:4]1[CH:5]=[C:6]([N+:11]([O-:13])=[O:12])[C:7]([NH2:10])=[C:8]([I:15])[CH:9]=1

Komponenten

5

Edukt 2

HCID 807IodineHCID 3941008Methyl 4-amino-3-nitrobenzoate

Produkt 1

HCID 67512142Methyl 4-amino-3-iodo-5-nitrobenzoateAusbeute 66 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 159865Silver sulfateKatalysatorHCID 702EthanolLösungsmittel

Versuchsvorschrift

To a solution of 4-amino-3-nitro-benzoic acid methyl ester (4.6 g, 23.45 mmol) in ethanol (120 mL) was added iodine (8.33 g, 32.83 mmol), followed by Ag2SO4 (10.24 g 32.83 mmol). The mixture was stirred overnight at room temperature and then filtered. The filtrate was concentrated under reduced pressure and the residue was purified by column chromatography to give 4.98 g (66%) of 4-amino-3-iodo-5-nitro-benzoic acid methyl ester.

Aufarbeitung

  1. filtrationfiltered
  2. concentrationThe filtrate was concentrated under reduced pressure
  3. customthe residue was purified by column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-820e441be93a41d5adf6e33c87e3f570
Quelldatensatz
uspto-grants-2016_09
Patentnummer
US09440956B2

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