Reaktion #2389094

ord-a1fbca80a68742168f9738b613b55c2c

Lösungsmittel

Reaktionsbedingungen

Temperatur
180°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturAfter cooled
  2. 2
    Sonstigepurified by silica gel column chromatography (eluent; methylene chloride:methanol=30:1 v/v)
  3. 3
    Sonstigerecrystallized from a mixed solvent of n-hexane-ethyl acetate

Vorschrift

386 mg of 3-nitrophthalic anhydride and 242 mg of (R)-α-methylbenzylamine were charged in an egg-plant type flask of 50 ml, followed by stirring under heating at a temperature of 180° C. for 1.5 hours. After cooled, the reaction product was dissolved in chloroform, purified by silica gel column chromatography (eluent; methylene chloride:methanol=30:1 v/v), recrystallized from a mixed solvent of n-hexane-ethyl acetate, to obtain 430 mg of the desired product as a light yellow powder. Yield: 73%. m.p. 115-117° C.; MS(EI+) 296(M)+

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06429212B1uspto-grants-2002_08