Reaktion #66952

ord-7f7f6d236f294044bd0244302e538dad

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturat reflux for 17 hours
  2. 2
    Sonstigeto reach room temperature
  3. 3
    Sonstigesolvent was evaporated to dryness
  4. 4
    WaschenResidue was washed with EtOH
  5. 5
    Filtrationa yellowish solid was filtered

Vorschrift

In a 500 mL round-bottom flask a mixture of 3-aminopyrazole (Aldrich, 10 g, 120 mmol) and phthalic anhydride (Aldrich, 24.96 g, 168 mmol) in 1,4-dioxane (150 mL) was stirred at reflux for 17 hours. The reaction was allowed to reach room temperature and solvent was evaporated to dryness. Residue was washed with EtOH and a yellowish solid was filtered to afford 23.6 g (yield 92%) of the title compound. 1H NMR (300 MHz, DMSO-d6) δ ppm: 13.09 (br s, 1H), 7.89-7.98 (m, 4H), 7.86 (br s, 1H), 6.36 (d, 1H). [ES+MS] m/z 214 (MH+).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08524750B2uspto-grants-2013_09