(E)-1-Phenyl-1,3-butadiene → HCID 14328884, 화합물

HRID 867961

반응식

HRID 867961 반응식
[N:1]1([CH2:6][C:7]([C:11]2[CH:20]=[CH:19][C:18]3[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=3)[CH:12]=2)=[N+:8]([O-:10])[CH3:9])[CH:5]=[CH:4][N:3]=[CH:2]1.[C:21]1(/[CH:27]=[CH:28]/[CH:29]=[CH2:30])[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1>C1(C)C=CC=CC=1>[N:1]1([CH2:6][C:7]2([C:11]3[CH:20]=[CH:19][C:18]4[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=4)[CH:12]=3)[CH2:30][CH:29](/[CH:28]=[CH:27]/[C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[O:10][N:8]2[CH3:9])[CH:5]=[CH:4][N:3]=[CH:2]1

참가 물질

4

반응물 2

HCID 5371758(E)-1-Phenyl-1,3-butadieneHCID 867424722-(1H-Imidazol-1-yl)-N-methyl-1-(2-naphthalenyl)ethanimine N-oxide

생성물 1

HCID 14328884HCID 14328884, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
85 °C

실험 절차

A mixture of compound 2 (11.02 g, 0.042 mol) and trans-1-phenyl-1,3-butadiene (8.0 g, 0.062 mol) in 500 ml of toluene is heated to 85° C. and held there for 72 hours, cooled and evaporated to dryness. The oil that remained is purified by flash chromatography on silica gel (eluent comprised of 98% CHCl3 and 2% MeOH by volume). The resulting semisolid is dissolved in chloroform, decolorized with carbon, and filtered through a bed of celite. The solvent is evaporated and the resulting tan solid recrystallized from ethyl acetate/hexane, m.p. 166°-169° C. (Found: C, 78.68; H, 6.39; N, 10.60. C26H25N3O requires: C, 78.96; H, 6.37; N, 10.62).

후처리

  1. temperaturecooled
  2. customevaporated to dryness
  3. customThe oil that remained is purified by flash chromatography on silica gel (eluent comprised of 98% CHCl3 and 2% MeOH by volume)
  4. dissolutionThe resulting semisolid is dissolved in chloroform
  5. filtrationfiltered through a bed of celite
  6. customThe solvent is evaporated
  7. customthe resulting tan solid recrystallized from ethyl acetate/hexane, m.p. 166°-169° C. (Found: C, 78.68; H, 6.39; N, 10.60. C26H25N3O requires: C, 78.96; H, 6.37; N, 10.62)

출처 및 근거

ORD 기록
ord-5272098743274c4c9b009b20f811903e
출처 데이터셋
uspto-grants-1988_10
특허 번호
US04777263

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