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Phenol → 2-Chloro-4,6-diphenoxy-1,3,5-triazine

HRID 1066445
ノート
印刷プレビュー

反応式

HRID 1066445 の反応式
[N:1]1[C:8](Cl)=[N:7][C:5](Cl)=[N:4][C:2]=1[Cl:3].[C:10](=[O:13])(O)[O-].[Na+].[C:15]1(C)[CH:20]=[CH:19]C=[CH:17][CH:16]=1.[C:22]1([OH:28])[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1>C(OCC)(=O)C.O>[Cl:3][C:2]1[N:4]=[C:5]([O:28][C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[N:7]=[C:8]([O:13][C:10]2[CH:19]=[CH:20][CH:15]=[CH:16][CH:17]=2)[N:1]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 996PhenolHCID 1140TolueneHCID 7954Cyanuric chlorideHCID 516892Sodium Bicarbonate

生成物 1

HCID 180882-Chloro-4,6-diphenoxy-1,3,5-triazine

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8857
Ethyl Acetate
溶媒

実験手順

A 2-liter reaction flask equipped with a magnetic stirrer and a condenser is charged with 92.2 g (0.50 mol) of cyan uric chloride, 84 g (1.0 mol) of sodium bicarbonate and 400 mL of toluene. The suspension is brought to 50° C. and 94 g (1.0 mol) of phenol are added in small portions. The mixture is refluxed for ten hours and then allowed to cool to room temperature. Portions of water and ethyl acetate (300 mL each) are added and the mixture is then filtered. The phases are separated and the organic phase is dried over anhydrous magnesium sulfate. The solvent is removed under reduced pressure to afford 150 g of crude product. The crude product is twice recrystallized from toluene to yield 48.7 g of the title compound as a white powder melting at 117-121° C.

後処理

  1. customA 2-liter reaction flask
  2. customequipped with a magnetic stirrer and a condenser
  3. customis brought to 50° C.
  4. temperatureThe mixture is refluxed for ten hours
  5. filtrationthe mixture is then filtered
  6. customThe phases are separated
  7. dry with materialthe organic phase is dried over anhydrous magnesium sulfate
  8. customThe solvent is removed under reduced pressure
  9. customto afford 150 g of crude product
  10. customThe crude product is twice recrystallized from toluene

出典と根拠

ORDレコード
ord-9c6dd437f70e4cac82d080d47971ec22
出典データセット
uspto-grants-2001_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06242598B1

反応ノート

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