Results of multistage copolymerization of phenylacetylenes (1st stage: 1, 2nd stage: 2) with a Rh-based multicomponent catalyst system using initiator Aa.
| run | [1]/([A]/3) | [2]/([A]/3) | Polymer | |||
|---|---|---|---|---|---|---|
| Sample code | Yieldb (%) | M n × 10−4c | M w/Mnc | |||
| 4 | 50 | 50 | A(poly(150-b-250))3 | 94 | 2.9 | 1.05 |
| 5 | 250 | 250 | A(poly(1250-b-2250))3 | 85 | 9.3 | 1.35 |
a
Reaction conditions: A (0.10 mmol), [Rh(nbd)Cl]2 (0.067 mmol), DPA (0.2 mmol), in THF (0.2 mL) at 0 °C for 10 min, then phenylacetylene (1) (1.7 mmol (run 4), 8.5 mmol (run 5)) and PPh3 (0.2 mmol) in THF (3.8 mL) at 30 °C for 20 min. Then, monomer (2) (1.7 mmol (run 4), 8.5 mmol (run 5)) was added.
b
Methanol-insoluble part.
c
Determined by SEC using three columns (TSKgel G4000HXL + G3000HXL + G3000HXL) connected in series (run 4) or one column (KF-805L) (run 5) based on polystyrene standards (THF, 40 °C).