Table 4. Copolymerization of MPDL with hydrophilic monomers by ICAR ATRP.
Entry | M1/M2/I/CuBr2/L/RI | M1 | Time, h | M̄n | M̄w/M̄n | fMPDL, % | RO, % |
---|---|---|---|---|---|---|---|
| |||||||
1 | 200/100/1/0.03/0.06/0.1 | OEOA480 | 10.7 | 31 | 1.07 | 20.5 | 32 |
2 | 1000/500/1/0.15/0.3/0.5 | OEOA480 | 10 | 50 | 1.37 | 9.2 | 62 |
3 | 1000/500/1/0.15/0.3/0.25 | OEOMA500 | 10 | 147 | 1.73 | 6.1 | 82 |
4 | 1000/500/1/0.75/1.5/0.25 | OEOMA500 | 6 | 125 | 1.49 | 5.9 | 74 |
5 | 150/150/1/0.03/0.06/0.1 | PEOMA2k | 13 | 52 | 1.08 | 6.0 | 96 |
Volume – 5 ml total; reaction solvent – DMF; T = 90 °C; M1 – BA, M2 – MPDL; L – Me6TREN; [I] = [EBiB] = 5 mM; RI – radical initiator: V40 (Tt1/2=10h = 88 °C); entries 1–2: [M1] = 1 M, [M2] = 0.5 M; entry 5: [M1] = 0.3 M, [M2] = 0.3 M; RO – % of MPDL monomer in ring-opened form to ring-closed form; fMPDL – fraction of MPDL incorporated into the polyether backbone, final M̄n was measured by DMF GPC with MALLS detector.