Reaktion #448509

ord-d2979447f54640189cffabeb4a769559

Reaktionsbedingungen

Temperatur
100°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstige(approximately one minute)
  2. 2
    TemperaturThe reaction mixture was cooled
  3. 3
    workup.WAITplaced in an ice bath for a half hour
  4. 4
    FiltrationThe crystallized product was filtered
  5. 5
    Waschenwashed well with diethyl ether, and air
  6. 6
    Sonstigedried

Vorschrift

4-Amino-3-pyridinol (3.3 g) was added to 1-piperidinylformamide dimethyl acetal (50 ml) and the mixture was stirred at 100° C. until it became homogeneous (approximately one minute). The reaction mixture was cooled, and placed in an ice bath for a half hour. The crystallized product was filtered, washed well with diethyl ether, and air dried to yield 4.64 g of product. This was recrystallized from ethyl acetate and dried under high vacuum and refluxing ethanol overnight to yield 3.39 g of fluffy needles, m.p. 171°-172.5° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05866565uspto-grants-1999_02