Cyanuric chloride → N,N',N''-trioctadecyl-1,3,5-triazine-2,4,6-triamine

HRID 40424

반응식

HRID 40424 반응식
[CH2:1]([NH2:19])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18].COCCCO[CH2:26][CH2:27][CH2:28]OC.[C:31]([O-])(=O)[CH3:32].[Na+].[N:36]1[C:43](Cl)=[N:42][C:40](Cl)=[N:39][C:37]=1Cl>CC(O)C.C(O)(=O)C>[CH2:1]([NH:19][C:37]1[N:39]=[C:40]([NH:19][CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18])[N:42]=[C:43]([NH:19][CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:31][CH2:32][CH2:28][CH2:27][CH3:26])[N:36]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18]

참가 물질

7

반응물 4

HCID 7954Cyanuric chlorideHCID 15793OctadecylamineHCID 863021-Methoxy-3-(3-methoxypropoxy)propaneHCID 517045Sodium Acetate

생성물 1

HCID 21758268N,N',N''-trioctadecyl-1,3,5-triazine-2,4,6-triamine

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 3776Isopropanol용매

반응 조건

온도
85 °C

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.

후처리

  1. temperatureto reflux out of the reaction mixture
  2. temperatureThe reaction mixture was heated to 170° C. for sixteen hours
  3. temperaturehad cooled to 80° C
  4. filtrationThe precipitate was filtered at room temperature
  5. washwashed with excess 2-propanol
  6. stirringThe solid was stirred
  7. temperaturein refluxing water (2.00 liters) for two hours
  8. filtrationfiltered
  9. washwashed with excess water
  10. stirringThe solid was stirred
  11. temperaturein refluxing 2-propanol (2.00 liters)
  12. filtrationfiltered
  13. washwashed with excess 2-propanol

출처 및 근거

ORD 기록
ord-c1c824e4b36c4c7fa0cf2336fe534b7b
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08529671B2

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