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

HRID 635892

반응식

HRID 635892 반응식
[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

참가 물질

4

반응물 2

HCID 7954Cyanuric chlorideHCID 178420626HCID 178420626, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

(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.

후처리

  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

출처 및 근거

ORD 기록
ord-fa5b09b24dba42f1bbcdaec160dd76b1
출처 데이터셋
uspto-grants-2001_02
특허 번호
US06191149B1

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