Reaktion #433188

Reaktionsgleichung

diethylenetriamine

NaOH

monochloro

2-Chloro-4-[N-(2,2,6,6-tetramethyl-4piperidyl)-n-butylamino]-6-(2,2,6,6-tetramethyl-4-hexyloxypiperidin-1yl)-1,3,5-triazine

→

N,N',N"-Tris{2-(2,2,6,6-tetramethyl-4-hexyloxypiperidin-1-yl)-4-[N-(2,2,6,6-tetramethylpiperidin-4-yl)-butylamino]-1,3,5-triazin-6-yl}-diethylenetriamine

Lösungsmittel

water

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturAfter warming to 100°
2. 2
   workup.DISTILLATIONto distill off
3. 3
   workup.ADDITIONA further 50 ml of toluene and 1 g of polyethylene glycol 1000 and 0.9 g of NaOH are added
4. 4
   Temperaturthe mixture is heated
5. 5
   Temperaturunder reflux
6. 6
   TemperaturAfter cooling
7. 7
   workup.ADDITIONthe reaction mixture is diluted
8. 8
   Waschenthe solution is washed four times with water
9. 9
   TrocknenThe organic solution is dried over Na2SO4
10. 10
    Sonstigeevaporated
11. 11
    workup.DISSOLUTIONThe residue is dissolved in 50 ml of methanol
12. 12
    Filtrationfiltered through 200 g of silica gel
13. 13
    Waschenwashed with 500 ml of methanol
14. 14
    SonstigeThe methanol solution is evaporated

Vorschrift

0.71 ml of diethylenetriamine and 0.9 g of NaOH, dissolved in 3 ml of water, are added to 10.6 g of the monochloro derivative from Example 70, dissolved in 50 ml of toluene. After warming to 100°, the solvent begins to distill off. A further 50 ml of toluene and 1 g of polyethylene glycol 1000 and 0.9 g of NaOH are added and the mixture is heated with stirring for 14 h under reflux. After cooling, the reaction mixture is diluted using 100 ml of ethyl acetate and the solution is washed four times with water. The organic solution is dried over Na2SO4 and evaporated. The residue is dissolved in 50 ml of methanol, filtered through 200 g of silica gel and washed with 500 ml of methanol. The methanol solution is evaporated, the residue being a nearly colorless resin.

Quelle