Reaktion #1869191

ord-b6144c65f26f4ab9b05a510cb7e2755e

Lösungsmittel

Reaktionsbedingungen

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

Aufarbeitung

  1. 1
    workup.STIRRINGThe reaction was then stirred at 0° C. for 30 minutes
  2. 2
    Sonstigewas quenched with glacial AcOH (2.5 ml)
  3. 3
    SonstigeThe solvent was removed in vacuo

Vorschrift

3-Hydroxy-2-nitropyridine (20 g, 0.143 mole) was dissolved in methanol (400 ml) and a solution of 25% sodium methoxide in methanol (33 ml, 0.13 mol) was added at room temperature. The mixture was stirred for 30 minutes, then cooled to 0° C., and bromine (7.2 ml, 0.14 mol) was added slowly. The reaction was then stirred at 0° C. for 30 minutes, then was quenched with glacial AcOH (2.5 ml). The solvent was removed in vacuo to afford material (30 g, 96%), which was used without further purification.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07498326B2uspto-grants-2009_03