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

HRID 1583921
ノート
印刷プレビュー

反応式

HRID 1583921 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 7954Cyanuric chlorideHCID 8143OctylamineHCID 14797Potassium Hydroxide

生成物 1

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

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

反応条件

温度
40 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-342977f1428543b290e0bc67d2afc5da
出典データセット
uspto-grants-1985_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04555479

反応ノート

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