Table 1.
Entrya | Time | 1:3:4b | Yield of 3c |
---|---|---|---|
1 | 10 min × 2 | 0:1:trace | 45 |
2 | 10 min × 3 | 0:1:trace | 49 |
3 | 15 min × 2 | 0:1:trace | 48 |
4 | 15 min | 11:50:1 | n/a |
5 | 20 min | 0:1:trace | 57 |
6 | 30 min | 0:1:trace | 57 |
7 | 45 min | 0:1:trace | 56 |
8 | 60 min | 0:1:trace | 56 |
9 mol % PdCl2(dppf)CH2Cl2, THF:H2O (10:1) at 0.051 M, 5 equiv of 2, 3 equiv Cs2CO3, 150 °C.
Determined by 1H NMR integration of the crude mixture.
Isolated yield.