2,6-Difluoroaniline → 2,6-Bis[(2,6-difluorophenylimino)-(phenyl) methyl]pyridine

HRID 1841514

反応式

HRID 1841514 の反応式
[C:1]([C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([C:15](=O)[C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[N:10]=1)(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[F:23][C:24]1[CH:30]=[CH:29][CH:28]=[C:27]([F:31])[C:25]=1[NH2:26]>C1(C)C=CC=CC=1>[F:23][C:24]1[CH:30]=[CH:29][CH:28]=[C:27]([F:31])[C:25]=1[N:26]=[C:15]([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)[C:11]1[CH:12]=[CH:13][CH:14]=[C:9]([C:1](=[N:26][C:25]2[C:24]([F:23])=[CH:30][CH:29]=[CH:28][C:27]=2[F:31])[C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[N:10]=1

参加物

4

反応物 2

HCID 796472,6-DifluoroanilineHCID 3166562,6-Dibenzoylpyridine

生成物 1

HCID 206142932,6-Bis[(2,6-difluorophenylimino)-(phenyl) methyl]pyridine

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

2,6-Dibenzoylpyridine (464 mg, 1.61 mmol) and 2,6-difluoroaniline (7.33 mg, 5.67 mmol) were dissolved in 30 ml of toluene. To this solution molecular sieves (4 Å) were added. After standing for 3 days at room temperature (with addition of more molecular sieves after 2 days) the mixture was filtered. The solvent was removed in vacuo. The residue was crystallised from ethanol. Yield 250 mg (30%) of 2,6-bis[(2,6-difluorophenylimino) (phenyl) methyl]pyridine 8 as a mixture of 3 isomers.

後処理

  1. additionTo this solution molecular sieves (4 Å) were added
  2. addition(with addition of more molecular sieves after 2 days) the mixture
  3. filtrationwas filtered
  4. customThe solvent was removed in vacuo
  5. customThe residue was crystallised from ethanol
  6. additionYield 250 mg (30%) of 2,6-bis[(2,6-difluorophenylimino) (phenyl) methyl]pyridine 8 as a mixture of 3 isomers

出典と根拠

ORDレコード
ord-7cd8931326e3491992238fcde8fe45f0
出典データセット
uspto-grants-2004_01
特許番号
US06683187B2

関連ノート

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