Reacción #68702

Ecuación de reacción

octadecylamine

di(propylene glycol) dimethyl ether

sodium acetate

cyanuric chloride

→

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

Disolventes

acetic acid

2-Propanol

Condiciones de reacción

Tratamiento posterior

1. 1
   Temperaturato reflux out of the reaction mixture
2. 2
   TemperaturaThe reaction mixture was heated to 170° C. for sixteen hours
3. 3
   Temperaturahad cooled to 80° C
4. 4
   FiltraciónThe precipitate was filtered at room temperature
5. 5
   Lavadowashed with excess 2-propanol
6. 6
   workup.STIRRINGThe solid was stirred
7. 7
   Temperaturain refluxing water (2.00 liters) for two hours
8. 8
   Filtraciónfiltered
9. 9
   Lavadowashed with excess water
10. 10
    workup.STIRRINGThe solid was stirred
11. 11
    Temperaturain refluxing 2-propanol (2.00 liters)
12. 12
    Filtraciónfiltered
13. 13
    Lavadowashed with excess 2-propanol

Procedimiento

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.

Fuente