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Cyanuric chloride → 6-Chloro-N~2~,N~4~-dioctyl-1,3,5-triazine-2,4-diamine

HRID 1583921
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HRID 1583921 반응식
[N:1]1[C:8]([Cl:9])=[N:7][C:5](Cl)=[N:4][C:2]=1Cl.[CH2:10]([NH2:18])[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17].[OH-].[K+]>CC(C)=O>[CH2:10]([NH:18][C:2]1[N:1]=[C:8]([Cl:9])[N:7]=[C:5]([NH:18][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17])[N:4]=1)[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17]
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참가 물질

5

반응물 3

HCID 7954Cyanuric chlorideHCID 8143OctylamineHCID 14797Potassium Hydroxide

생성물 1

HCID 183563846-Chloro-N~2~,N~4~-dioctyl-1,3,5-triazine-2,4-diamine수율 64.9%

시약·촉매·용매 1

HCID 180Acetone용매

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온도
40 °C

실험 절차

37 g (0.2 mol) of cyanuric chloride was dissolved in 80 ml of hot acetone and the solution was rapidly added to 120 ml of ice water (crushed ice:water=1:1) with vigorous stirring. The temperature reached 0° to 5° C. 56.8 g (0.44 mol) of n-octylamine was gradually added dropwise while maintaining the temperature at 10° C. or below. Then, the temperature was raised to 40° C. by heating and the mixture was heated on a water bath for 1 hour. Since the pH of the reaction solution turned into the acid region (pH<2), granules of potassium hydroxide was gradually added to maintain the pH around neutral (the time required was 1 hour). The product deposited in the reaction solution was cooled and separated by filtration. The crystals were thoroughly washed with water and dried. The crude crystals were recrystallized from ethanol to obtain 48 g of Intermediate A having a melting point of 171°-172° C.

후처리

  1. customreached 0° to 5° C
  2. temperaturewhile maintaining the temperature at 10° C. or below
  3. temperatureby heating
  4. temperaturethe mixture was heated on a water bath for 1 hour
  5. additionwas gradually added
  6. temperatureto maintain the pH around neutral (the time
  7. temperaturewas cooled
  8. customseparated by filtration
  9. washThe crystals were thoroughly washed with water
  10. customdried
  11. customThe crude crystals were recrystallized from ethanol

출처 및 근거

ORD 기록
ord-342977f1428543b290e0bc67d2afc5da
출처 데이터셋
uspto-grants-1985_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04555479

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