Reaktion #726871

ord-b5b3896dfb60434e8d941b1f41fcee64

Lösungsmittel

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONAfter the addition
  2. 2
    Sonstigethe ice bath was removed
  3. 3
    Temperaturto warm to room temperature over 16 h
  4. 4
    workup.ADDITIONIce was added to the mixture
  5. 5
    Sonstigeto provide a precipitate, which
  6. 6
    Filtrationwas collected by filtration
  7. 7
    Sonstigedried in vacuo

Vorschrift

6-Chloro-2,4-dihydroxy-5-methyl-pyridine (500 mg, 3.1 mmol) was taken up in acetic acid (1 mL), cooled to 0° C. and nitric acid added (4 mL) dropwise with stirring. After the addition was complete, the ice bath was removed, and the reaction mixture was allowed to warm to room temperature over 16 h. Ice was added to the mixture to provide a precipitate, which was collected by filtration and dried in vacuo to give the title compound as a yellow solid (180 mg, 28%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07691877B2uspto-grants-2010_04