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

HRID 49751

반응식

HRID 49751 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
50 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-5cf68a390d7c4ef1aa9f36af3a6e1ed9
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06710006B2

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