Water → 2,5-Dibromo-3-nitropyridine

HRID 538572

Reaktionsgleichung

Reaktionsgleichung von HRID 538572
[Br:1][C:2]1[CH:3]=[C:4]([N+:9]([O-:11])=[O:10])[C:5](O)=[N:6][CH:7]=1.P(Br)(Br)[Br:13].O>C1(C)C=CC=CC=1.CN(C=O)C>[Br:13][C:5]1[C:4]([N+:9]([O-:11])=[O:10])=[CH:3][C:2]([Br:1])=[CH:7][N:6]=1

Komponenten

6

Edukt 3

HCID 962WaterHCID 24614Phosphorus tribromideHCID 178418997HCID 178418997, Verbindung

Produkt 1

HCID 2984702,5-Dibromo-3-nitropyridineAusbeute 80,03 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 1140TolueneLösungsmittelHCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

To a solution of 5-Bromo-3-nitro-pyridin-2-ol (10.0 g, 45.66 mmol) in 70 ml of toluene and 7 ml of DMF was added PBr3 (6.60 ml, 68.49 mmol) and the reaction mixture was heated at 120° C. for 20 min under nitrogen atmosphere. After the completion of the reaction mixture (TLC monitoring), water (100 mL) was added and extracted with ethyl acetate (3×200 mL). The combined organics was washed with water, brine, dried (Na2SO4), filtered and concentrated to get the desired product (10.30 g, 80.03%).

Aufarbeitung

  1. extractionextracted with ethyl acetate (3×200 mL)
  2. washThe combined organics was washed with water, brine
  3. dry with materialdried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-393084f0690840619769a6aea28260a2
Quelldatensatz
uspto-grants-2014_10
Patentnummer
US08865736B2

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