Reaktion #433179

ord-766a6fc445b14e6f83e1a5aa8451b644

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONare added
  2. 2
    TemperaturAfter cooling
  3. 3
    Sonstigethe phases are separated
  4. 4
    TrocknenThe organic phase is dried over Na2SO4
  5. 5
    Sonstigeevaporated
  6. 6
    SonstigeRecrystallizing from acetonitrile leads to the compound of the above structure which melts at 154°-156° (white powder)

Vorschrift

3.8 g of morpholine and, 15 minutes later, a solution of 1.7 g of NaOH in 5 ml of water are added to a solution of 30 g of 2,4-dichloro-6-(4,4-ethylenedioxy-2,2,6,6-tetramethylpiperidin-1-yl)-1,3,5-triazine (product from Example 17) in 100 ml of toluene. The mixture is then warmed to 6020 and after 45 minutes a further 3.8 g of morpholine and 1.7 g of NaOH in 5 ml of water are added. After a further 1.5 hours, the reaction has ended. After cooling and adding 200 ml of toluene, the phases are separated. The organic phase is dried over Na2SO4 and evaporated. Recrystallizing from acetonitrile leads to the compound of the above structure which melts at 154°-156° (white powder).

Quelle

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