Реакция #68702

Уравнение реакции

octadecylamine

di(propylene glycol) dimethyl ether

sodium acetate

cyanuric chloride

→

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

Растворители

acetic acid

2-Propanol

Условия реакции

Обработка

1. 1
   Температураto reflux out of the reaction mixture
2. 2
   ТемператураThe reaction mixture was heated to 170° C. for sixteen hours
3. 3
   Температураhad cooled to 80° C
4. 4
   ФильтрацияThe precipitate was filtered at room temperature
5. 5
   Промывкаwashed with excess 2-propanol
6. 6
   workup.STIRRINGThe solid was stirred
7. 7
   Температураin refluxing water (2.00 liters) for two hours
8. 8
   Фильтрацияfiltered
9. 9
   Промывкаwashed with excess water
10. 10
    workup.STIRRINGThe solid was stirred
11. 11
    Температураin refluxing 2-propanol (2.00 liters)
12. 12
    Фильтрацияfiltered
13. 13
    Промывкаwashed with excess 2-propanol

Методика

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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