Reaktion #645649

ord-47f0014f41424e53bb949261e0874928

Reaktionsbedingungen

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

Aufarbeitung

  1. 1
    SonstigeThe tube was sealed
  2. 2
    Temperaturthe solution was cooled to RT
  3. 3
    Einengenconcentrated in vacuo
  4. 4
    SonstigeThe residue was purified by reverse phase chromatography (neutral)

Vorschrift

To a resealable pressure vessel charged with 3-bromo-2-chloro-4-picoline (1.200 g, 5.81 mmol) was added formic acid (13.1 ml, 348 mmol) and water (4.00 ml, 222 mmol). The tube was sealed and the solution heated to 120° C. After 72 hrs, the solution was cooled to RT and concentrated in vacuo. The residue was purified by reverse phase chromatography (neutral) to afford 3-bromo-4-methylpyridin-2(1H)-one as a white solid. M+H+=188.0.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08063055B2uspto-grants-2011_11