Cyanuric chloride → 2,4-Dichloro-6-phenyl-1,3,5-triazine

HRID 635892ノート

反応式

HRID 635892 の反応式
[Cl:1][C:2]1[N:7]=[C:6]([Cl:8])[N:5]=[C:4](Cl)[N:3]=1.[C:10]1([Mg]Br)[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.O1CCCC1>O1CCCC1>[Cl:1][C:2]1[N:7]=[C:6]([Cl:8])[N:5]=[C:4]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[N:3]=1

参加物

4

反応物 2

HCID 7954Cyanuric chlorideHCID 178420626HCID 178420626、化合物

生成物 1

HCID 155492,4-Dichloro-6-phenyl-1,3,5-triazine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

(Step 1) To 50 g of 2,4,6-trichloro-1,3,5-triazine was added 300 ml of dry tetrahydrofuran and while the mixture was stirred at room temperature, 150 ml of 2M phenylmagnesium bromide-tetrahydrofuran was added dropwise over about 30 minutes. After completion of dropwise addition, the mixture was stirred at room temperature for 1 hour, and then concentrated. To the residue was added iced water and the resultant was extracted with ether. The extract was washed with water, dried over MgSO4, and concentrated. The resulting crystal crop was recrystallized from isopropyl alcohol to provide 21.1 g of 2,4-dichloro-6-phenyl-1,3,5-triazine as pale yellow crystals.

後処理

  1. additionAfter completion of dropwise addition
  2. stirringthe mixture was stirred at room temperature for 1 hour
  3. concentrationconcentrated
  4. additionTo the residue was added iced water
  5. extractionthe resultant was extracted with ether
  6. washThe extract was washed with water
  7. dry with materialdried over MgSO4
  8. concentrationconcentrated
  9. customThe resulting crystal crop was recrystallized from isopropyl alcohol

出典と根拠

ORDレコード
ord-fa5b09b24dba42f1bbcdaec160dd76b1
出典データセット
uspto-grants-2001_02
特許番号
US06191149B1

反応ノート

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