2-Fluoroaniline → 2-[1-(2,4,6-Trimethylphenylimino) ethyl]-6-[1-(2-fluorophenylimino)ethyl]pyridine

HRID 49751

反応式

HRID 49751 の反応式
[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[C:4]([CH3:9])[C:3]=1[N:10]=[C:11]([C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([C:19](=O)[CH3:20])[N:14]=1)[CH3:12].[F:22][C:23]1[CH:29]=[CH:28][CH:27]=[CH:26][C:24]=1[NH2:25]>C1(C)C=CC=CC=1>[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[C:4]([CH3:9])[C:3]=1[N:10]=[C:11]([C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([C:19](=[N:25][C:24]2[CH:26]=[CH:27][CH:28]=[CH:29][C:23]=2[F:22])[CH3:20])[N:14]=1)[CH3:12]

参加物

4

反応物 2

HCID 95842-FluoroanilineHCID 221344681-{6-[(1E)-N-(2,4,6-Trimethylphenyl)ethanimidoyl]pyridin-2-yl}ethan-1-one

生成物 1

HCID 213000492-[1-(2,4,6-Trimethylphenylimino) ethyl]-6-[1-(2-fluorophenylimino)ethyl]pyridine

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
50 °C

実験手順

Monoimine (1, 1.0 g, 3.57 mmol) and 2-fluoroaniline (398 mg, 3.57 mmol) (ex. Aldrich) were dissolved in 50 ml of toluene. To this solution, 4 Å molecular sieves were added. After standing for 20 hrs., with addition of more molecular sieves, the mixture was filtered. The solvent was removed in vacuum and the oily residue was warmed in ethanol (50° C.). The yellow solid, which precipitated after cooling at −20° C., was filtered off and dried in vacuo. Yield 300 mg (23%) of mixed diimine (4).

後処理

  1. additionTo this solution, 4 Å molecular sieves were added
  2. addition, with addition of more molecular sieves
  3. filtrationthe mixture was filtered
  4. customThe solvent was removed in vacuum
  5. customThe yellow solid, which precipitated
  6. temperatureafter cooling at −20° C.
  7. filtrationwas filtered off
  8. customdried in vacuo

出典と根拠

ORDレコード
ord-5cf68a390d7c4ef1aa9f36af3a6e1ed9
出典データセット
uspto-grants-2004_03
特許番号
US06710006B2

関連ノート

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