Tridentate ligand-contg. metal catalyst complexes for olefin polymerization
A technology of catalysts and complexes, applied in the direction of iron group organic compounds without C-metal bonds, 7/17 group organic compounds without C-metal bonds, 4/14 group organic compounds without C-metal bonds, etc. Ability to address issues such as potential utility of unsuggested compounds
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Embodiment 1
[0063] [(Ph 2 PCH 2 SiMe 2 ) 2 N]TiCl 2 (1) Synthesis
[0064] To (Ph 2 PCH 2 SiMe 2 ) 2 To a solution of NH (0.500 g, 0.944 mmol) in pentane (15 ml) was added 1.6M BuLi in hexane (0.59 ml, 0.94 mmol). Upon addition, a white precipitate formed and the mixture was stirred at room temperature for 30 minutes. The solid was allowed to settle and the solvent was removed by pipette. The solid was washed with pentane (10ml) then dissolved in thf (10ml). The thf solution was added dropwise to TiCl 3 • 3thf (0.350g, 0.944mmol) in suspension in thf (30ml). When added, the color changes from light blue to olive green. After stirring at room temperature for 16 hours, the volatiles were removed under reduced pressure and the residue was extracted with toluene (30ml). The dark green solution was filtered through Celite(R), concentrated to 10 mL, and cooled to -30°C. The product was isolated as gray-green crystals (0.291 g, 0.449 mmol, 48%). Elemental analysis, IR spectrum, a...
Embodiment 2
[0066] [(Ph 2 PCH 2 SiMe 2 ) 2 N] VCl 2 (2) Synthesis
[0067] From VCl as described for Ti derivatives in Example 1 3 3thf (0.353g, 0.944mmol) and (Ph 2 PCH 2 SiMe 2 ) 2 NH (0.500 g, 0.944 mmol) synthesized the compound. The product was isolated from toluene / pentane as dark red crystals. Yield 0.415 g (0.638 mmol, 68%). Elemental analysis, IR spectroscopy, magnetic moment, and X-ray crystallographic data were consistent with the title compound.
Embodiment 3
[0069] [(Ph 2 PCH 2 SiMe 2 ) 2 N]CrCl 2 Synthesis of (thf)(3)
[0070] From CrCl as described for Ti derivatives in Example 1 3 3thf (0.707g, 1.89mmol) and (Ph 2 PCH 2 SiMe 2 ) 2 NH (1.00 g, 1.89 mmol) synthesized the compound. The product was isolated from toluene / pentane as magenta crystals. One molecule of thf is coordinated to the metal. Yield 0.644g (0.890mmol, 47%). Elemental analysis, IR spectroscopy, magnetic moment, and X-ray crystallographic data were consistent with the title compound.
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