Hydrochloric Acid → 5-Bromo-2-iodopyridin-3-ol

HRID 661102Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 661102
O.C(=O)([O-])[O-].[Na+].[Na+].[Br:8][C:9]1[CH:10]=[N:11][CH:12]=[C:13]([OH:15])[CH:14]=1.O.[I:17]I.Cl>>[Br:8][C:9]1[CH:14]=[C:13]([OH:15])[C:12]([I:17])=[N:11][CH:10]=1

Komponenten

6

Edukt 5

HCID 313Hydrochloric AcidHCID 807IodineHCID 962WaterHCID 5995293-Bromo-5-hydroxypyridineHCID 2735133Sodium Carbonate Monohydrate

Produkt 1

HCID 226029855-Bromo-2-iodopyridin-3-olAusbeute 99,4 %

Versuchsvorschrift

To a mixture of sodium carbonate monohydrate (1.96 mL, 35.5 mmol) and 3-bromo-5-hydroxypyridine (2.06 g, 11.8 mmol) in H2O (0.213 mL, 11.8 mmol) was added iodine crystals (0.640 mL, 12.4 mmol), and the overall mixture was stirred at room temperature overnight. The mixture was then poured slowly into 2M HCl(aq), and the pH was adjusted to ˜3. The product was collected by filtration followed by crystallization from EtOH/water to afford 5-bromo-2-iodopyridin-3-ol as an off-white solid of (3.53 g, 99.4% yield) m/z (%): 301.2 (100%, M++H).

Aufarbeitung

  1. filtrationThe product was collected by filtration
  2. customfollowed by crystallization from EtOH/water

Quellen und Nachweise

ORD-Eintrag
ord-1a5407e86b4140a59bfae67480841bd8
Quelldatensatz
uspto-grants-2011_12
Patentnummer
US08084479B2

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