Reaktion #68536

ord-fbc2170a0cad4978b70181a962d4c39c

Lösungsmittel

Reaktionsbedingungen

Temperatur
245°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeA two-necked round bottomed flask equipped with an air condenser
  2. 2
    Temperaturwas cooled to RT
  3. 3
    Filtrationfiltered
  4. 4
    Sonstigeto obtain a dark solid
  5. 5
    Filtrationfiltered
  6. 6
    Sonstigeto obtain product as a brown solid

Vorschrift

A two-necked round bottomed flask equipped with an air condenser was charged with 5-[(5-Methoxy-pyridin-3-ylamino)-methylene]-2,2-dimethyl-[1,3]dioxane-4,6-dione (18 g) and diphenyl ether (180 mL). The reaction mixture was heated at 240-250° C. for 5 min under N2 atmosphere after which it was cooled to RT, diluted with hexane and filtered to obtain a dark solid. The crude product was refluxed in hexane for 30 min and filtered to obtain product as a brown solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08524900B2uspto-grants-2013_09