Hydrochloric Acid → 6-Chloro-2-iodo-3-hydroxypyridine

HRID 269584Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 269584
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([OH:8])=[CH:4][CH:3]=1.C(=O)([O-])[O-].[Na+].[Na+].[I:15]I.Cl>O>[Cl:1][C:2]1[N:7]=[C:6]([I:15])[C:5]([OH:8])=[CH:4][CH:3]=1

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 807IodineHCID 10340Sodium CarbonateHCID 8198212-Chloro-5-hydroxypyridine

Produkt 1

HCID 234331586-Chloro-2-iodo-3-hydroxypyridine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

6-Chloro-3-pyridinol (2.0 g, 15.44 mmol) was stirred in water (40 ml) containing sodium carbonate (3.43 g, 32.36 mmol) and iodine (3.92 g, 15.44 mmol) was added. The mixture was stirred at room temperature for 72 hours. The pH was adjusted to pH8 with 1M hydrochloric acid solution and the mixture extracted with ethyl acetate (×2). The combined organic extracts were washed with brine and dried (MgSO4). The aqueous layer was acidified to pH5 with 1M hydrochloric acid solution and extracted with ethyl acetate, which was washed with brine, dried (MgSO4) and the combined solutions evaporated to leave the title compound as a buff solid (3.70 g).

Aufarbeitung

  1. additionwas added
  2. extractionthe mixture extracted with ethyl acetate (×2)
  3. washThe combined organic extracts were washed with brine
  4. dry with materialdried (MgSO4)
  5. extractionextracted with ethyl acetate, which
  6. washwas washed with brine
  7. dry with materialdried (MgSO4)
  8. customthe combined solutions evaporated

Quellen und Nachweise

ORD-Eintrag
ord-fda67ea3df394f178adaaec59d622444
Quelldatensatz
uspto-grants-2008_11
Patentnummer
US07446222B2

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