Reaktion #433172

ord-c7bb789d0b1d4f4bacfa19354d6ade46

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe mixture is subsequently heated
  2. 2
    Temperaturto reflux
  3. 3
    Sonstigefor 26 hours
  4. 4
    Temperaturto cool
  5. 5
    Filtrationthe precipitate is filtered off
  6. 6
    SonstigeThe filtrate is evaporated in vacuo
  7. 7
    SonstigeThe residue is recrystallized from 300 ml of acetonitrile
  8. 8
    SonstigeThe product obtained

Vorschrift

A solution of 55.3 g (0.3 mol) of cyanuric chloride in 300 ml of xylene is added dropwise with stirring and cooling to 0°-5° to a solution of 119.6 g (0.6 mol) of 4,4-ethylenedioxy-2,2,6,6-tetramethylpiperidine in 100 ml of xylene. The mixture is subsequently heated to reflux and kept at boiling point for 26 hours. After addition of 150 ml of xylene, the mixture is allowed to cool and the precipitate is filtered off. The filtrate is evaporated in vacuo. The residue is recrystallized from 300 ml of acetonitrile. The product obtained is a brownish powder which melts at 169°-172°.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05059689uspto-grants-1991_10