Table 1. Copolymerization of BA with MPDL by ICAR ATRP.
Entry | M1/M2/I/CuBr2/L/RI | T, °C | Conv., % | Time, h | Mnth | M̄n | M̄w/M̄n | fMPDL, % | RO, % |
---|---|---|---|---|---|---|---|---|---|
| |||||||||
1 | 100/50/1/0.015/0.03/0.1 | 65 | 55 | 9.7 | 10 320 | 5 400 | 1.35 | 29.9 | 35 |
2 | 100/50/1/0.015/0.03/0.1 | 88 | 52 | 6 | 11 030 | 4 820 | 1.39 | 23.4 | 46 |
3 | 100/50/1/0.015/0.03/0.1 | 110 | 46 | 2 | 9 800 | 4 360 | 1.41 | 26.4 | 55 |
[M1] = [BA] = 1 M, [M2] = [MPDL] = 0.5 M, [I] = [EBiB] = 10 mM, 10 ml total; L – Me6TREN; reaction solvent – DMF; RI – radical initiator: entry 1 – AIBN (Tt1/2=10h = 65 °C), entry 2– V40 (Tt1/2=10h = 88°C), entry 3– Vam110 (Tt1/2=10h = 110 °C); RO – % of MPDL monomer in ring-opened form to ring-closed form; Mnth – theoretical mass, fMPDL – fraction of MPDL incorporated into the p(BA) backbone, monomer conversion was measured by 1H NMR; M̄n and M̄w was obtained by THF GPC with PMMA calibration standards.