تفاعل #586080

ord-bf7af8a743ed4c7cba15bc741b3b5637

معادلة التفاعل

CCCCCCCCCCCCCCCCCCN
octadecylamine
COCCCOCCCOC
di(propylene glycol) dimethyl ether
CC(=O)[O-].[Na+]
sodium acetate
Clc1nc(Cl)nc(Cl)n1
cyanuric chloride
CCCCCCCCCCCCCCCCCCNc1nc(NCCCCCCCCCCCCCCCCCC)nc(NCCCCCCCCCCCCCCCCCC)n1
N,N′,N″-trioctadecyl-1,3,5-triazine-2,4,6-triamine

المذيبات

ظروف التفاعل

درجة الحرارة
85°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةto reflux out of the reaction mixture
  2. 2
    درجة الحرارةThe reaction mixture was heated to 170° C. for sixteen hours
  3. 3
    درجة الحرارةhad cooled to 80° C
  4. 4
    ترشيحThe precipitate was filtered at room temperature
  5. 5
    غسيلwashed with excess 2-propanol
  6. 6
    workup.STIRRINGThe solid was stirred
  7. 7
    درجة الحرارةin refluxing water (2.00 liters) for two hours
  8. 8
    ترشيحfiltered
  9. 9
    غسيلwashed with excess water
  10. 10
    workup.STIRRINGThe solid was stirred
  11. 11
    درجة الحرارةin refluxing 2-propanol (2.00 liters)
  12. 12
    ترشيحfiltered
  13. 13
    غسيلwashed with excess 2-propanol

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07765698B2uspto-grants-2010_08