Reaktion #66293

ord-469bd8986c634922893dbc45d4e96c95

Reaktionsgleichung

COC(=O)c1ccccc1O
methyl 2-hydroxybenzoate
CCCN
n-propylamine
CCCNC(=O)c1ccccc1O
2-hydroxy-N-propylbenzamide
Ausbeute 84.0%

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    EinengenThe reaction mixture was concentrated under reduced pressure
  2. 2
    Sonstigeto give the crude material that
  3. 3
    Sonstigewas purified by silica gel flash column chromatography

Vorschrift

The crude methyl 2-hydroxybenzoate was dissolved in n-propylamine (400 mL). The reaction mixture in a sealed reactor was stirred at 80° C. overnight. The reaction mixture was concentrated under reduced pressure to give the crude material that was purified by silica gel flash column chromatography to afford 120 g (84%) of 2-hydroxy-N-propylbenzamide. LCMS ESI (+) m/z 180 (M+1) detected.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08524702B2uspto-grants-2013_09