Table 1.
| ||
---|---|---|
Entry |
Change from initial conditions[b] |
Yield of 2 a [%][c] |
1 |
no change |
54 |
2 |
nBu4NBr (c=0.3 mol l −1) as conducting salt[d] |
55 |
3 |
I =8 mA [e] |
72 |
4 |
I=6.5 mA or 5 mA |
71 |
5 |
I=2.5 mA |
43 |
6 |
T=0 °C |
36 |
7 |
T=40 °C |
41 |
8 |
c(nBu4NBr)=0.2 mol l −1 |
60 |
[a] Reactions were performed in a divided cell on a 0.25 mmol scale with a substrate concentration of 36 mmol l −1. [b] Initial conditions: 3.0 equiv TMSCl, 0.3 mol l −1 nBu4NClO4, DMF, 23 °C, 10 mA, 2.0 F mol−1, CuSn17Pb (leaded bronze) cathode, graphite anode. [c] Yield determined by GLC of the unpurified reaction mixture with mesitylene as internal standard. [d] This change was kept for entries 3–7. [e] This change was kept for entries 6–8.