Reaktion #433176

ord-9fbad73837c84bddab7d6e029b6b2c74

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe internal temperature being maintained at 10°
  2. 2
    SonstigeThe phases are separated
  3. 3
    Waschenthe organic phase is washed with water
  4. 4
    Trocknendried over Na2SO4
  5. 5
    Sonstigeevaporated
  6. 6
    SonstigeAfter recrystallizing from hexane
  7. 7
    Sonstigethe above product is produced as a white powder which melts at 114°-116° C.

Vorschrift

43.4 g of 2,4-dichloro-6-(2,2,6,6-tetramethylpiperidin-1-yl)-1,3,5-triazine (product from Example 1) are dissolved in 175 ml of toluene, after which 42.1 g of pulverized KOH, 1 g of potassium carbonate and 3.4 g of tetrabutylammonium hydrogen sulfate are added. A solution of 29.9 g of 1-acetyl-2,2,6,6-tetramethyl-4-hydroxy-piperidine in 110 ml of toluene is then added dropwise, the internal temperature being maintained at 10° using an ice bath. After stirring for 3.5 hours, 100 ml of water are added. The phases are separated, and the organic phase is washed with water, dried over Na2SO4 and evaporated. After recrystallizing from hexane, the above product is produced as a white powder which melts at 114°-116° C.

Quelle

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