Potassium Iodide → HCID 178524773, Verbindung

HRID 488462

Reaktionsgleichung

Reaktionsgleichung von HRID 488462
[OH:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][N:3]=1.[I:11]([O-])(=O)=O.[K+].[I-].[K+]>O.OS(O)(=O)=O>[OH:1][C:2]1[C:10]([I:11])=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][N:3]=1

Komponenten

6

Edukt 3

HCID 4875Potassium IodideHCID 23665710Potassium IodateHCID 178418479HCID 178418479, Verbindung

Produkt 1

HCID 178524773HCID 178524773, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 1118Sulfuric AcidLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

6-Hydroxynicotinic acid (20 g) in water (200 ml) and H2SO4 (80 ml) was heated to 90° C. for 1 hour. Potassium iodate (0.42 equivalent) and potassium iodide (0.96 equivalent) were both added portionwise over 2 hours. After a further hour at 90° C. the mixture was cooled to 60° C. and added to 1 kg of ice. The brown solid was filtered off, dried and taken up in DMF (30 ml)/EtOH(1 litre). Sodium metabisulfite was added until the brown colour disappeared and the mixture was poured onto ice (2 kg), a further 1.5 litre water added and the white solid filtered to give title compound (16.5 g). NMR δ(DMSO) 12.95 (1H, broad), 12.35 (1H, broad), 8.36 (1H, d), 8.03 (1H, d)

Aufarbeitung

  1. additionboth added portionwise over 2 hours
  2. filtrationThe brown solid was filtered off
  3. customdried
  4. additionSodium metabisulfite was added until the brown colour
  5. additionthe mixture was poured onto ice (2 kg)
  6. additiona further 1.5 litre water added
  7. filtrationthe white solid filtered

Quellen und Nachweise

ORD-Eintrag
ord-4d1cf850ac544cdda7fec36221f94862
Quelldatensatz
uspto-grants-2005_12
Patentnummer
US06972297B2

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