Hydrochloric Acid → 2-Bromo-6-iodopyridin-3-ol

HRID 506768

Reaktionsgleichung

Reaktionsgleichung von HRID 506768
[I:1]I.[Br:3][C:4]1[C:9]([OH:10])=[CH:8][CH:7]=[CH:6][N:5]=1.C([O-])([O-])=O.[K+].[K+].Cl>O>[Br:3][C:4]1[C:9]([OH:10])=[CH:8][CH:7]=[C:6]([I:1])[N:5]=1

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 807IodineHCID 11430Potassium CarbonateHCID 230702-Bromo-3-pyridinol

Produkt 1

HCID 109794792-Bromo-6-iodopyridin-3-ol

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

Add I2 (21.0 g, 82.7 mmol) in solid form, a little at a time, in the space of 5 min, to a solution of 2-bromo-3-pyridinol (14.0 g, 80.8 mmol) and of K2CO3 (22.3 g, 161 mmol) in H2O (180 mL). Stir the reaction medium at room temperature for 2 h, then cool it (ice/H2O) to 0-5° C. and neutralize it to pH 6 by adding 2N HCl. A precipitate forms, which is filtered, washed with H2O and dried under vacuum at 70° C. to give 2 (19.48, 80.7%) in solid form, of an ivory color: 1H NMR (CDCl3) δ 7.54 (d, 1H, J=8.1 Hz), 6.98 (d, 1H, J=8.1 Hz), 5.55 (s broad, 1H); m/z obs.=299.4 (M+1).

Aufarbeitung

  1. customin the space of 5 min
  2. filtrationA precipitate forms, which is filtered
  3. washwashed with H2O
  4. customdried under vacuum at 70° C.
  5. customto give 2 (19.48, 80.7%) in solid form

Quellen und Nachweise

ORD-Eintrag
ord-33b95e27c7d94a8d9410943d817b2973
Quelldatensatz
uspto-grants-2010_08
Patentnummer
US07786114B2

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