Table 3. Effect of Chelating Phosphine Ligands.
Entry | Ligand | Bite Angle(c) | 2 | 3a | 4 | 5a |
---|---|---|---|---|---|---|
1 | dppm | 7329a | 12 | 11 | 51 | 26 |
2 | dppe-p-CF3 | 86(d) | 20 | 25 | 28 | 27 |
3(g) | dppe | 8629a | 5 | 7 | 63 | 25 |
4 | dppe-p-OMe | 86(d) | 3 | 4 | 69 | 24 |
5 | dpp-benzene | 87(e),29b | 87 | 3 | 7 | 4 |
6 | dcpe | 8729c | 11 | 4 | 19 | 66 |
7 | dppp | 9129a | 31 | 58 | 8 | 3 |
8 | BINAP | 9329d | 32 | 9 | 37 | 22 |
9(g) | dppb | 9429e | 4 | 10 | 56 | 30 |
10 | dppf | 9929f | 27 | 42 | 12 | 19 |
11 | dppf-i-Pr | 10329g | 13 | 12 | 0 | 75 |
12 | dpe-phos | 104(f),29h | 19 | 27 | 37 | 17 |
13 | xantphos | 108(f),29h | 54 | 46 | 0 | 0 |
Conditions: 1.0 equiv 1a, 2.0 equiv 4-bromotoluene, 1.2 equiv NaOtBu, 1 mol % Pd2(dba)3, 2 mol % ligand, toluene (0.25 M), 110 °C. The product ratios refer to GC ratios of products 2-5 that have been corrected for GC response factor. All reactions proceed to completion unless otherwise noted.
The reaction was conducted with 1.4 equiv 4-bromotoluene.
Bite angles were obtained from crystal structures of bis(phosphine)PdCl2 complexes.
The bite angle was estimated based on analogy to dppe.
The bite angle was obtained from a crystal structure of the bis(phosphine)PdBr2 complex.
The bite angle was obtained from a crystal structure of the bis(phosphine)Pd(1,1-dimethylallyl)tetrafluoroborate complex.
Approximately 3% of an imine side product derived from substrate oxidation was detected by GC and GC/MS analysis of the crude reaction mixture.