Optimization of final Heck coupling.
| Entry | [Pd] (mol%) | Condition | Yield (%) |
|---|---|---|---|
| 1 | PdCl2(MeCN)2 (10) | Et3N, HCO2H, MeCN, rt, 3 h | Decomposition |
| 2 | Pd(PPh3)4 (5) | Et3N, Bu4NCl, DMF, rt, 6 h | Trace |
| 3 | PdCl2(PPh3)2 (10) | K2CO3, Bu4NCl, DMF, rt, 12 h | 10 |
| 4 | Pd(Oac)2 (5) | Et3N, Bu4NCl, DMF, rt, 4 h | 45′ |
| 5 | Pd(Oac)2 (5) | K3PO4, DMF, rt, 12 h | 40 |
| 6 | [Pd(μ-I)(PtBu3)]2 (7.5) | DIPEA, toluene, rt, 9 h | 58 |
| 7 | Pd(Oac)2, (10) Pd(PPh3)4 (10) | K3PO4, DMF, rt, 18 h | 77 |