Réaction #586080

Équation de réaction

octadecylamine

di(propylene glycol) dimethyl ether

sodium acetate

cyanuric chloride

→

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

Solvants

acetic acid

2-Propanol

Conditions de réaction

Traitement

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

Mode opératoire

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.

Source