Lanthanide oxaziazide complexes, catalytic systems comprising the same and processes for (co)polymerization of conjugated dienes
A catalytic system, conjugated diene technology, used in organic compound/hydride/coordination complex catalysts, chemical instruments and methods, physical/chemical process catalysts, etc.
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example 1
[0191] Synthesis of Ligands of Formula (L1)
[0192]
[0193] 5.37 ml (0.036 mol) of 2-tert-butylaniline were introduced into the reaction flask together with 15 ml of methanol and 5 drops of formic acid to obtain a solution. 30 ml of methanol containing 5.87 g (0.036 mol) of 2,6-diacetylpyridine was then added dropwise to the solution at room temperature, resulting in the precipitation of a yellow microcrystalline solid: the yellow solid was recovered by filtration, washed with cold methanol and in Drying under vacuum at room temperature afforded 9.84 g of a pale yellow solid of formula (L1) (Yield = 93%).
[0194] Elemental analysis [found (calculated)]: C: 78.0% (77.5%); H: 7.60% (7.53%); N: 9.65% (9.52%); O: 5.30% (5.43%).
[0195] Molecular weight (MW): 294.4.
[0196] FT-IR (liquid paraffin): 1694cm -1 v (C=O) 1644cm -1 v (C＝N) .
[0197] Figure 12 The obtained FT-IR (liquid paraffin) spectrum of the ligand of formula (L1) is shown.
example 2
[0199] Synthesis of Ligands of Formula (L2)
[0200]
[0201] 2.70 ml (0.014 moles) of 2,6-diisopropylaniline were introduced into the reaction flask together with 5 ml of methanol and 0.25 ml of formic acid to obtain a solution. 20 ml of methanol containing 1.93 g (0.012 mol) of 2,6-diacetylpyridine was then added dropwise to this solution at room temperature, resulting in the precipitation of a yellow microcrystalline solid: the yellow solid was recovered by filtration, washed with cold methanol and in Drying under vacuum at room temperature afforded 2.4 g of a whitish solid of formula (L2) (Yield = 62%).
[0202] Elemental analysis [found (calculated)]: C: 77.80% (78.22%); H: 8.24% (8.13%); N: 8.51% (8.69%); O: 4.91% (4.96%).
[0203] Molecular weight (MW): 322.45.
[0204] FT-IR (liquid paraffin): 1696cm -1 v (C＝O) 1645cm -1 v (C＝N) .
[0205] 1 H-NMR (delta shift from TMS): 1.16 (d, 12H), 2.27 (s, 3H), 2.73 (m, 2H), 2.80 (s, 3H), 7.17 (m, 3H), 7.95 (t, 1H), ...
example 3
[0207] Synthesis of Ligands of Formula (L3)
[0208]
[0209] 0.80 ml (0.0057 mol) of 2,4,6-trimethylaniline was introduced into the reaction flask together with 5 ml of methanol and 2 drops of formic acid to obtain a solution. 5 ml of methanol containing 0.937 g (0.0057 mol) of 2,6-diacetylpyridine was then added dropwise to this solution at room temperature, resulting in the precipitation of a yellow microcrystalline solid: the yellow solid was recovered by filtration, washed with cold methanol and in Drying under vacuum at room temperature afforded 1.2 g of a pale yellow solid of formula (L3) (yield = 75%).
[0210] Elemental analysis [found (calculated)]: C: 77.20% (77.11%); H: 7.20% (7.19%); N: 10.0% (9.99%), O: 5.60% (5.71%).
[0211] Molecular weight (MW): 280.36.
[0212] FT-IR (liquid paraffin): 1698cm -1 v (C＝O) 1637cm -1 v (C＝N) .
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