Block copolymerization of IP and CL with pre-catalyst 6a.
| ||||||||
|---|---|---|---|---|---|---|---|---|
| Entry | Feed ratio (IP : CL) | Conv.b (%) | M n c (kDa) | Đ c | Poly(1,3-diene) : polyesterd,e (%) | Microstructuree,fCis-1,4/Trans-1,4/3,4 | T g g , h (°C) | T m g , h (°C) |
| 1 | 800 : 300 | >99 | 110(21) | 1.10(2) | 68 : 32 | 51/48/1 | −66 | 51 |
| 2 | 550 : 550 | >99 | 90.9(17) | 1.12(1) | 47 : 53 | 44/54/2 | −67 | 55 |
| 3 | 300 : 800 | >99 | 101(20) | 1.23(3) | 26 : 74 | 28/70/2 | −64 | 54 |
Conditions: 6, 10 μmol; [Ph3C][B(C6F5)4], 10 μmol; toluene, 10 mL; room temperature; IP 12 h; CL 2 h; all entries are done in triplicate.
Determined by 1H NMR spectroscopy of crude reaction mixtures, comparing monomer peaks to polymer.
Determined by gel permeation chromatography (GPC) in THF using a Wyatt DAWN HELEOS II MALS detector.
Determined by 1H NMR spectroscopy of the isolated polymer.
Average of the triplicate runs.
1,4 and 3,4 selectivity determined by 1H NMR. Cis-1,4 and trans-1,4 selectivity determined by 13C NMR.
Determined by low temperature differential scanning calorimetry (DSC).
Data for one of the individual runs.