Water → 2-[4-(4,6-Bis-trichloromethyl-s-triazin-2-yl)benzoylmethylene]-1-methyl-1,2-dihydroquinoline

HRID 345198노트

반응식

HRID 345198 반응식
C(N(CC)CC)C.[CH3:8][N+:9]1[C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[CH:12]=[CH:11][C:10]=1[CH3:19].CC1C=CC(S(O)(=O)=O)=CC=1.[Cl:31][C:32]([Cl:53])([Cl:52])[C:33]1[N:38]=[C:37]([C:39]([Cl:42])([Cl:41])[Cl:40])[N:36]=[C:35]([C:43]2[CH:51]=[CH:50][C:46]([C:47](Cl)=[O:48])=[CH:45][CH:44]=2)[N:34]=1.O>C1(C)C=CC=CC=1.C(Cl)Cl>[Cl:42][C:39]([Cl:40])([Cl:41])[C:37]1[N:38]=[C:33]([C:32]([Cl:53])([Cl:31])[Cl:52])[N:34]=[C:35]([C:43]2[CH:44]=[CH:45][C:46]([C:47]([CH:19]=[C:10]3[CH:11]=[CH:12][C:13]4[C:18](=[CH:17][CH:16]=[CH:15][CH:14]=4)[N:9]3[CH3:8])=[O:48])=[CH:50][CH:51]=2)[N:36]=1

참가 물질

7

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 14473251HCID 14473251, 화합물HCID 86745141HCID 86745141, 화합물

생성물 1

HCID 867451422-[4-(4,6-Bis-trichloromethyl-s-triazin-2-yl)benzoylmethylene]-1-methyl-1,2-dihydroquinoline

시약·촉매·용매 2

HCID 1140Toluene용매HCID 6344Dichloromethane용매

실험 절차

Triethylamine (17.4 pbw) are added dropwise at 15° C. to 14.1 pbw of 1,2-dimethyl-quinolinium-p-toluenesulfonate and 22.2 pbw of 4-(4,6-bis-trichloromethyl-s-triazin-2-yl)-benzoylchloride in 150 ml of dried toluene. The mixture is then allowed to warm to room temperature. After 1 hour the mixture is poured onto 600 pbw of water, admixed with 600 pbw of methylene chloride and extracted by shaking. Silica gel (100 pbw) is added to the dried organic phase and the mixture is stirred for 30 minutes. The silica gel is removed by filtration and the solvents are distilled off in vacuo the residue is recrystallized from 2-methoxyethanol, giving strong red crystals.

후처리

  1. extractionextracted
  2. additionSilica gel (100 pbw) is added to the dried organic phase
  3. stirringthe mixture is stirred for 30 minutes
  4. customThe silica gel is removed by filtration
  5. distillationthe solvents are distilled off in vacuo the residue
  6. customis recrystallized from 2-methoxyethanol
  7. customgiving strong red crystals

출처 및 근거

ORD 기록
ord-8f45e78cd8554e72a11eefbbd6c96278
출처 데이터셋
uspto-grants-1991_10
특허 번호
US05055579

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