Phosphorus oxychloride → 2-Bromo-4-chloropyridin-3-ol

HRID 1846237Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1846237
[Br:1][C:2]1[C:7]([O:8]C)=[C:6]([Cl:10])[CH:5]=[CH:4][N:3]=1.P(Cl)(Cl)(Cl)=O.COC1C(=O)C=CNC=1Br>>[Br:1][C:2]1[C:7]([OH:8])=[C:6]([Cl:10])[CH:5]=[CH:4][N:3]=1

Komponenten

4

Edukt 3

HCID 24813Phosphorus oxychlorideHCID 497615912-Bromo-3-methoxypyridin-4-olHCID 866967432-Bromo-4-chloro-3-methoxypyridine

Produkt 1

HCID 722139992-Bromo-4-chloropyridin-3-ol

Reaktionsbedingungen

Temperatur
20 °C

Versuchsvorschrift

2-bromo-4-chloro-3-methoxypyridine. Phosphorus oxychloride (10 eq.) and 3-methoxy-2-bromo-4(1H)-pyridone (1 eq.) are stirred at 90° C. for 18 h, concentrated in vacuo, and cooled to 20° C. The residue is treated with ice water and adjusted to pH 12 with 40% NaOH, and the product is extracted into DCM. The residue obtained on evaporation of the combined extracts is distilled at reduced pressure to afford the title compound.

Aufarbeitung

  1. concentrationconcentrated in vacuo
  2. additionThe residue is treated with ice water
  3. extractionthe product is extracted into DCM
  4. customThe residue obtained on evaporation of the combined extracts
  5. distillationis distilled at reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-6f3984306a1c4420b795d126c90c0480
Quelldatensatz
uspto-grants-2015_02
Patentnummer
US08952009B2

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