反応 #1528392

ord-da3d6ae50f12465285d9389e6cc6deb2

反応方程式

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
収率 46.0%

反応条件

温度
4°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The suspension was heated
  2. 2
    温度to reflux
  3. 3
    ろ過filtered hot
  4. 4
    その他afforded yellow crystals, which
  5. 5
    ろ過were filtered
  6. 6
    洗浄washed with cold ligroin

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07655592B2uspto-grants-2010_02