Reaktion #70272

ord-a4e2c39a7efe46fa98d2f35b3345c17e

Lösungsmittel

Reaktionsbedingungen

Temperatur
120°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionextracted with DCM
  2. 2
    SonstigeThe crude mixture was purified by flash chromatography over SiO2 eluting with hexane/ethyl acetate

Vorschrift

A mixture of 3-bromo-5-nitropyridin-2-ol, POBr3 and PBr3 was heated at 120° C. for 3.5 h. The crude mixture was poured into a mixture of ice and water and extracted with DCM. The crude mixture was purified by flash chromatography over SiO2 eluting with hexane/ethyl acetate mixtures affording 2.63 g (yield 73%) of the expected product.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08536165B2uspto-grants-2013_09