반응 #433188

반응 방정식

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

용매

water

toluene

반응 조건

후처리

1. 1
   온도After 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
   온도the mixture is heated
5. 5
   온도under reflux
6. 6
   온도After cooling
7. 7
   workup.ADDITIONthe reaction mixture is diluted
8. 8
   세척the solution is washed four times with water
9. 9
   건조The organic solution is dried over Na2SO4
10. 10
    기타evaporated
11. 11
    workup.DISSOLUTIONThe residue is dissolved in 50 ml of methanol
12. 12
    여과filtered through 200 g of silica gel
13. 13
    세척washed with 500 ml of methanol
14. 14
    기타The methanol solution is evaporated

실험 절차

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.

출처