Table 3. Polymerization of rac-LA with, [LTH-M(OiPr)2] Initiators, Generated In Situ from the Reaction of [LTH-MCl2] Complexes and [LiOiPr].
runa | catalyst | T (°C) | conv.b (%) | Mnc (g mol–1) × 103 (calcd) | Mnd (g mol–1) × 103 (GPC) | PDId | Pre |
---|---|---|---|---|---|---|---|
1 | LiOiPr | 0 | 97.2 | 14.0 | 13.1 | 1.25 | 0.56 |
2 | LiOiPr | 25 | 96.4 | 13.9 | 8.94 | 1.25 | 0.54 |
3 | [LTHZn(OiPr)2] | 0 | 96.6 | 13.9 | 6.273 | 1.25 | 0.74 |
4 | [LTHPd(OiPr)2] | 0 | 96.3 | 13.9 | 8.564 | 1.25 | 0.61 |
5 | [LTHCd(OiPr)2] | 0 | 95.7 | 13.8 | 5.347 | 1.25 | 0.54 |
6 | [LTHZn(OiPr)2] | 25 | 96.2 | 13.9 | 5.400 | 1.25 | 0.58 |
7 | [LTHPd(OiPr)2] | 25 | 96.5 | 13.9 | 6.409 | 1.25 | 0.54 |
8 | [LTHCd(OiPr)2] | 25 | 95.4 | 13.8 | 4.358 | 1.25 | 0.54 |
Specifications: [catalyst] 0.0625 mmol; [rac-LA]/[LiOiPr]/[catalyst] 100:2:1; solvent (CH2Cl2) 5.00 mL; polymerization time 20 min.
Conversion rate (%) was determined by 1H NMR spectroscopy in the presence of tetralin.
Calculated using [{molecular weight of rac-LA} × {(mol concentration of used rac-LA)/(mol concentration of catalyst)}] × [conversion].
Determined by gel permeation chromatography (GPC) in chloroform, relative to the poly(methyl methacrylate) standard.