반응 #1528392

ord-da3d6ae50f12465285d9389e6cc6deb2

반응 방정식

CC(C)c1cccc(C(C)C)c1N1CC(=N)N(c2c(C(C)C)cccc2C(C)C)C1
1,3-bis(2,6-diisopropylphenyl)-iminoimidazoline
[Cl-].[Cl-].[Cl-].[Ti+3][CH]1C=CC=C1
cyclopentadienyltitanium trichloride
CCN(CC)CC
triethylamine
CC(C)c1cccc(C(C)C)c1N1CC(=N)N(c2c(C(C)C)cccc2C(C)C)C1.[Cl-].[Cl-].[Ti+2][CH]1C=CC=C1
1,3-bis(2,6-diisopropylphenyl)-iminoimidazoline cyclopentadienyl titanium dichloride
수율 46.0%

반응 조건

온도
4°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The suspension was heated
  2. 2
    온도to reflux
  3. 3
    여과filtered hot
  4. 4
    기타afforded yellow crystals, which
  5. 5
    여과were filtered
  6. 6
    세척washed with cold ligroin

실험 절차

To a suspension of 1,3-bis(2,6-diisopropylphenyl)-iminoimidazoline (2.03 g, 5.0 mmol) and cyclopentadienyltitanium trichloride (1.10 g, 5.0 mmol) in toluene (30 mL) was added triethylamine (0.8 mL, 5,7 mmol) at ambient temperature. After stiriring for 1 hour, the thick yellow-orange suspension was diluted with toluene (50 mL) and ligroin (120 mL). The suspension was heated to reflux and filtered hot. Cooling to approx. 4° C. afforded yellow crystals, which were filtered and washed with cold ligroin to give 1.34 g (46% yield) of NMR pure 1,3-bis(2,6-diisopropylphenyl)-iminoimidazoline cyclopentadienyl titanium dichloride.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07655592B2uspto-grants-2010_02