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

HRID 345198ノート

反応式

HRID 345198 の反応式
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

参加物

7

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 14473251HCID 14473251、化合物HCID 86745141HCID 86745141、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8f45e78cd8554e72a11eefbbd6c96278
出典データセット
uspto-grants-1991_10
特許番号
US05055579

反応ノート

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