Reaktion #586080

Reaktionsgleichung

octadecylamine

di(propylene glycol) dimethyl ether

sodium acetate

cyanuric chloride

→

N,N′,N″-trioctadecyl-1,3,5-triazine-2,4,6-triamine

Lösungsmittel

acetic acid

2-Propanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturto reflux out of the reaction mixture
2. 2
   TemperaturThe reaction mixture was heated to 170° C. for sixteen hours
3. 3
   Temperaturhad cooled to 80° C
4. 4
   FiltrationThe precipitate was filtered at room temperature
5. 5
   Waschenwashed with excess 2-propanol
6. 6
   workup.STIRRINGThe solid was stirred
7. 7
   Temperaturin refluxing water (2.00 liters) for two hours
8. 8
   Filtrationfiltered
9. 9
   Waschenwashed with excess water
10. 10
    workup.STIRRINGThe solid was stirred
11. 11
    Temperaturin refluxing 2-propanol (2.00 liters)
12. 12
    Filtrationfiltered
13. 13
    Waschenwashed with excess 2-propanol

Vorschrift

Under a nitrogen atmosphere, a mixture of octadecylamine (389 grams, 1.44 mol), di(propylene glycol) dimethyl ether (1.50 liters), sodium acetate (134 grams, 1.63 mol), and cyanuric chloride (88.4 grams, 0.479 mol) was stirred for thirty minutes and then heated to 85° C. for two hours. The reaction mixture was heated to 155° C. at which temperature acetic acid was allowed to reflux out of the reaction mixture. The reaction mixture was heated to 170° C. for sixteen hours. 2-Propanol (1.60 liters) was added to the reaction mixture when it had cooled to 80° C. The precipitate was filtered at room temperature and washed with excess 2-propanol. The solid was stirred in refluxing water (2.00 liters) for two hours, filtered, and washed with excess water. The solid was stirred in refluxing 2-propanol (2.00 liters), filtered, and washed with excess 2-propanol to yield 377 grams of N,N′,N″-trioctadecyl-1,3,5-triazine-2,4,6-triamine as a white solid.

Quelle