반응 #68702

반응 방정식

octadecylamine

di(propylene glycol) dimethyl ether

sodium acetate

cyanuric chloride

→

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

용매

acetic acid

2-Propanol

반응 조건

후처리

1. 1
   온도to reflux out of the reaction mixture
2. 2
   온도The reaction mixture was heated to 170° C. for sixteen hours
3. 3
   온도had cooled to 80° C
4. 4
   여과The precipitate was filtered at room temperature
5. 5
   세척washed with excess 2-propanol
6. 6
   workup.STIRRINGThe solid was stirred
7. 7
   온도in refluxing water (2.00 liters) for two hours
8. 8
   여과filtered
9. 9
   세척washed with excess water
10. 10
    workup.STIRRINGThe solid was stirred
11. 11
    온도in refluxing 2-propanol (2.00 liters)
12. 12
    여과filtered
13. 13
    세척washed with excess 2-propanol

실험 절차

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.

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