Table 1.
Entry | Deviation from Standard Conditions | Yield (%)b | |||
---|---|---|---|---|---|
1 | 2 | 3 | 4 | ||
1 | None | 3 | 5 | 89 | 3 |
2 | 5% v/v H2O | 54 | 11 | 38 | 29 |
3 | No L1 or L2 | 83 | 43 | 7 | 0 |
4 | No NiBr2 • 3 H2O | 98 | 60 | 0 | 0 |
5 | No NiBr2 • 3 H2O, reverse current for 0.2 F/mol beforehand | 1 | 8 | 69 | 5 |
6 | No DIPEA | >99 | 68 | 0 | 0 |
7 | 0 F/molc | 99 | 93 | 0 | 0 |
8 | RVC instead of Ni foam and graphite | 45 | 17 | 41 | 18 |
9 | Graphite instead of Ni foam | 13 | 26 | 8 | 29 |
10 | 0.7 mA/cm2 instead of 1.3 mA/cm2 | 0 | 2 | 80 | 11 |
11 | 2.0 mA/cm2 instead of 1.3 mA/cm2 | 0 | 0 | 78 | 12 |
12 | 45 °C instead of 70 °C | 35 | 16 | 35 | 31 |
13 | LiBr instead of TBAPF6 | 3 | 0 | 66 | 10 |
Ni foam cathode surface area = 7.5 cm2.
Corrected GC yield vs dodecane.
Reaction mixture was stirred and heated for 4.3 h (length of reaction for 4 F/mol at 1.3 mA/cm2).