Table 1.
Entry | Initial ratioa | Time (h) | solvent | Concb (M) | M/Ic | Calc Mwd (g mol−1) | Polymer ratioe | Convf | Mng (NMR) | Mn (SEC) | Yield | PDI |
---|---|---|---|---|---|---|---|---|---|---|---|---|
1 | 10/1 | 48 | THF | 2.75 | 55 | 9930 | Na | 50% | Na | Na | Na | Na |
2 | 10/1 | 48 | CH2Cl2 | 2.75 | 55 | 9930 | 10/1 | 98% | 8670 | 13300 | 85% | 1.55 |
3 | 10/1 | 96 | CH2Cl2 | 1.38 | 55 | 9930 | 10/1 | 96% | 7050 | 22700 | 73% | 1.19 |
4 | 10/1 | 24 | CH2Cl2 | 2.75 | 55 | 9930 | 10/1 | 85% | 8530 | 7850 | 54% | 1.44 |
5 | 10/1 | 48 | CH2Cl2 | 2.50 | 55 | 9930 | 9/1 | 95% | 9200 | 11900 | 81% | 1.25 |
6 | 20/1 | 48 | CH2Cl2 | 2.75 | 63 | 10400 | 19/1 | 92% | 9340 | 11000 | 75% | 1.15 |
7h | 10/1 | 115 | CH2Cl2 | 2.75 | 110 | 19600 | 11/1 | 95% | 18700 | 88400 | 68% | 1.24 |
8h | 20/1 | 115 | CH2Cl2 | 3.15 | 126 | 20500 | 16/1 | 91% | 16200 | 69100 | 82% | 1.21 |
9 | 10/1 | 72 | CH2Cl2 | 2.75 | 110 | 19600 | 9/1 | 91% | 14600 | 22700 | 80% | 1.30 |
Lactide to molecule 7 ratio in the polymerizations.
Concentration of the monomers.
Ratio of the sum of the monomers to initiator.
Calculated molecular weight based on the ratio of monomers to initiator.
Observed ratio of lactide to molecule 7 in the copolymer as shown by 1H NMR spectroscopy.
Conversion of the polymerization.
The Mn was calculated from by end group analysis using 1H NMR spectroscopy.
The temperature of polymerization was 40 °C for these experiments, it was 35 °C for all other polymerizations.