Reaktion #433180

Reaktionsgleichung

diethanolamine

NaOH

diethanolamine

NaOH

2-chloro-4-morpholino-6-(4,4-ethylenedioxy-2,2,6,6-tetramethylpiperidin-1-yl)-1,3,5-triazine

2-Chloro-4-morpholino-6-(4,4-ethylenedioxy-2,2,6,6-tetramethylpiperidin-1-yl)-1,3,5-triazine

product

2-Chloro-4-morpholino-6-(4,4-ethylenedioxy-2,2,6,6-tetramethylpiperidin-1-yl)-1,3,5-triazine

→

2-[Bis-(2-hydroxyethyl)-amino]-4-morpholino-6-(4,4-ethylenedioxy-2,2,6,6-tetramethylpiperidin-1-yl)-1,3,5-triazine

Lösungsmittel

water

water

xylene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturunder reflux
2. 2
   workup.STIRRINGafter which the mixture is stirred
3. 3
   Temperaturunder reflux for a further 28 hours
4. 4
   Temperaturto cool
5. 5
   Waschenwashed with water
6. 6
   Sonstigethe organic phase is separated off
7. 7
   TrocknenAfter drying over Na2SO4
8. 8
   Sonstigeevaporating
9. 9
   Sonstigerecrystallizing twice from toluene
10. 10
    Sonstigethe above product is obtained as a white powder which melts at 135°-140°

Vorschrift

5.3 g of diethanolamine and a solution of 1 g of NaOH in 3 ml of water are added to a solution of 20 g of 2-chloro-4-morpholino-6-(4,4-ethylenedioxy-2,2,6,6-tetramethylpiperidin-1-yl)-1,3,5-triazine (product from Example 44) in 50 ml of xylene. 1 g of NaOH in 3 ml of water is again added after 1.75 hours with stirring under reflux. After 14 hours, 7.9 g of diethanolamine are added, after which the mixture is stirred under reflux for a further 28 hours. It is then allowed to cool and washed with water, and the organic phase is separated off. After drying over Na2SO4, evaporating and recrystallizing twice from toluene, the above product is obtained as a white powder which melts at 135°-140°.

Quelle