Table 2.
Entry | Init. 1 | M/ROH | Time (min) |
Conv. 2 (%) |
DP/OH 3 Calc. |
DP/OH 4 Final |
Init Eff. 5 % |
DM 6 |
---|---|---|---|---|---|---|---|---|
1 7 | DIC | 30 | 60 | 4 | - | - | - | |
2 | DIC | 10 | 30 | 94 | 9.4 | 14 | 67 | 1.10 |
3 8 | β-CD | 10 | 30 | 97 | 9.7 | 10 | 97 | 1.09 |
4 | DIC | 2 | 10 | 83 | 1.65 | 2.7 | 61 | 1.13 |
5 | DIC | 20 | 60 | 96 | 19.2 | 24.1 | 80 | 1.14 |
6 | AIC | 2 | 10 | 47 | 0.95 | 1.2 | 79 | 1.14 |
7 | α-CD | 10 | 10 | 97 | 9.6 | 11.2 | 86 | 1.07 |
8 | α-CD | 30 | 20 | 99 | 19.8 | 20.3 | 98 | 1.09 |
9 | γ-CD | 2 | 10 | 97 | 1.9 | 2.2 | 88 | 1.18 |
10 | γ-CD | 10 | 30 | 96 | 9.6 | 10.8 | 89 | 1.09 |
11 | 2,6-DM | 30 | 60 | 99 | 29.8 | ca. 80 | 37 | 1.49 |
12 | 2,3-DM | 10 | 30 | 96 | 9.6 | 9.6 | 100 | 1.34 |
1 DIC = DMAP/β-CD inclusion complex, AIC = adamantane/β-CD inclusion complex. 2 Conversion determined by 1H NMR (see experimental section). 3 Number-average degree of polymerization per initiating hydroxyl group calculated considering the growth of one macromolecular chain per hydroxyl group. 4 Number-average degree of polymerization per initiating hydroxyl group measured by 1H NMR (see experimental section). 5 Relative amount (%) of the cyclodextrin OH groups that initiate the growth of a macromolecular chain calculated as follows: (DP/OH calc)/(DP/OH final)*100. 6 Dispersity measured by size exclusion chromatography (THF, 40 °C, PS standards, chromatograms given in the SI Section Figures S4–S13). 7 Blank experiment conducted with the sole DMAP/β-CD inclusion complex, without additional DMAP catalyst. 8 Taken from ref [23].