反応 #433179

ord-766a6fc445b14e6f83e1a5aa8451b644

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONare added
  2. 2
    温度After cooling
  3. 3
    その他the phases are separated
  4. 4
    乾燥The organic phase is dried over Na2SO4
  5. 5
    その他evaporated
  6. 6
    その他Recrystallizing from acetonitrile leads to the compound of the above structure which melts at 154°-156° (white powder)

実験手順

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).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05059689uspto-grants-1991_10