Table 1.
Entry | Temp, °C | Monomer/initiator/Cu | [Cu], ppm | Ligand/ratio to Cu | AIBN/Initiator | Time, min | Conv., % |
Mn |
Mw/Mn | |
---|---|---|---|---|---|---|---|---|---|---|
Theoretical | GPC | |||||||||
1 | 60 | 200 St/1/0.01 | 50 | Me6TREN/1 | 0.1 | 2,760 | 44 | 8,700 | 7,900 | 1.12 |
2 | 60 | 200 St/1/0.01 | 50 | TPMA/1 | 0.1 | 2,880 | 39 | 7,800 | 6,800 | 1.09 |
3 | 60 | 200 St/1/0.01 | 50 | PMDETA/1 | 0.1 | 2,880 | 29 | 5,600 | 4,500 | 1.62 |
4 | 60 | 200 St/1/0.01 | 50 | dNbpy/2 | 0.1 | 2,940 | 36 | 7,200 | 5,600 | 1.68 |
5 | 70 | 200 St/1/0.01 | 50 | Me6TREN/1 | 0.1 | 2,400 | 47 | 9,500 | 7,600 | 1.11 |
6 | 70 | 200 St/1/0.01 | 50 | Me6TREN/1 | 0.2 | 2,500 | 60 | 11,900 | 10,000 | 1.15 |
7 | 70 | 200 St/1/0.01 | 50 | Me6TREN/1 | 0.4 | 1,140 | 66 | 13,200 | 10,100 | 1.22 |
8 | 110 | 200 St/1/0.01 | 50 | Me6TREN/10 | — | 1,775 | 65 | 12,900 | 11,000 | 1.25 |
9 | 110 | 200 St/1/0.01 | 50 | TPMA/10 | — | 1,930 | 49 | 9,800 | 9,600 | 1.13 |
10 | 110 | 200 St/1/0.002 | 10 | TPMA/50 | — | 1,720 | 42 | 8,400 | 7,600 | 1.38 |
11 | 110 | 200 St/1/0.0002 | 1 | TPMA/500 | — | 1,700 | 55 | 11,000 | 8,400 | 1.72 |
12 | 60 | 200 MMA/1/0.01 | 50 | TPMA/1 | 0.1 | 1,120 | 50 | 10,100 | 11,100 | 1.23 |
13 | 65 | 200 BA/1.25/0.01 | 50 | TPMA/1 | 0.01 | 1,910 | 35 | 7,100 | 8,900 | 1.46 |
Boldface numbers emphasize the variable of interest in a series of experiments. Ratios are molar. AIBN, azobisisobutyronitrile; GPC, gel-permeation chromatography; EtBrPA, ethyl α-bromophenylacetate. [St]0/[EtBrIB]0 = 200; [St]0 = 5.82 M; 50% anisole by volume; [BA]0/[EtBrIB]0 = 160; [BA]0 = 5.88 M; 20% anisole by volume; [MMA]0/[EtBrPA]0 = 200; [MMA]0 = 6.23 M; 50% anisole by volume.