Sodium Carbonate → HCID 178422452, Verbindung

HRID 1924950Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1924950
[CH3:1][C:2]1[N:7]=[C:6]([OH:8])[CH:5]=[C:4](O)[CH:3]=1.P(Br)(Br)([Br:12])=O.C([O-])([O-])=O.[Na+].[Na+]>CN(C=O)C.O>[Br:12][C:4]1[CH:3]=[C:2]([CH3:1])[N:7]=[C:6]([OH:8])[CH:5]=1

Komponenten

6

Edukt 3

HCID 10340Sodium CarbonateHCID 24613Phosphorus oxybromideHCID 178429093HCID 178429093, Verbindung

Produkt 1

HCID 178422452HCID 178422452, VerbindungAusbeute 46,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
110 °C

Versuchsvorschrift

A solution of 6-methylpyridine-2,4-diol (1.75 g, 14.0 mmol) in dry DMF (6.0 mL) is stirred under N2 and phosphorus oxybromide (3.05 g, 10.6 mmol) is added in one portion. The mixture is heated at 110° C. for 45 min and then cooled and diluted with water (7 mL). Na2CO3 (s) is added to bring the pH to 7 and the resulting suspension is cooled to 0° C. The product is collected by suction filtration, rinsing with cold water and diethyl ether, and dried overnight in a vacuum desiccator to afford the title compound as a light brown solid (920 mg).

Aufarbeitung

  1. temperaturecooled
  2. temperaturethe resulting suspension is cooled to 0° C
  3. filtrationThe product is collected by suction filtration
  4. washrinsing with cold water and diethyl ether
  5. customdried overnight in a vacuum desiccator

Quellen und Nachweise

ORD-Eintrag
ord-97f5a04ce55a4c4b89eeafb4f8161c54
Quelldatensatz
uspto-grants-2012_05
Patentnummer
US08178530B2

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