Table 1.
Polymerization of monomer 3a using ROMP
| entry | [M]o/[I] | catalyst | solvent[a] | temp (°C) |
time (h) |
conversion (%)[b] |
Yield[c,d] | Mntheo (g/mol) |
MnNMR
[e] (g/mol) |
MnGPC
[f] (g/mol) |
PDI[f] (Mn/Mw) |
|---|---|---|---|---|---|---|---|---|---|---|---|
| 1 | 100/1 | GII | CHCl3 | 20 | 4 | 84 | 72 | 23600 | 103800 | 63200 | 2.8 |
| 2 | 100/1 | GII | CHCl3 | 45 | 18 | 81[g] | 49 | 22800 | 26000 | 24900 | 2.6 |
| 3 | 25/1 | 5 | THF | 20 | 1 | 87 | 57 | 6100 | 6500 | 9300 | 1.4 |
| 4 | 50/1 | 5 | THF | 20 | 1 | 85 | 71 | 12000 | 12500 | 16300 | 1.4 |
| 5 | 100/1 | 5 | THF | 20 | 1 | 81 | 80 | 23100 | 22000 | 21600 | 1.4 |
| 6 | 100/1 | 5 | THF | 20 | 18 | 81 | 85 | 23100 | 22100 | 22300 | 1.4 |
| 7 | 200/1 | 5 | THF | 20 | 1 | 73 | 83 | 41000 | 45200 | 50300 | 1.5 |
[a]
[M]o = 1M.
[b]
based off of 1H-NMR integrations of monomer olefin signals to polymer olefin signals.
[c]
isolated.
[d]
theoretical yield based off of monomer conversion.
[e]
based off 1H-NMR integrations of polymers olefin signals and polymers chain-end phenyl signals.
[f]
calibrated with polystyrene standards, eluted in THF,
[g]
additional 10–15% cyclic dimer (see Supporting Information for structural characterization of byproduct).