Table 3.
Optimization of Reaction Conditions for Heteroaryl Chloridesa
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|---|---|---|---|---|
| entry | catalyst/ligand (mol %) | base | solvent (°C) | ratio 4a/3aa |
| 1 | Pd(OAc)2/XPhos (3/6) | K2CO3 | THF/H2O (80) | 72/28 |
| 2 | Pd(OAc)2/XPhos (3/6) | K2CO3 | CPME/H2O (100) | 77/23 |
| 3 | Pd(OAc)2/RuPhos (3/6) | Cs2CO3 | THF/H2O (80) | 46/54 |
| 4 | Pd(OAc)2/DavePhos (3/6) | Cs2CO3 | THF/H2O (80) | 0/100 |
| 5 | Pd(OAc)2/SPhos (3/6) | Cs2CO3 | THF/H2O (80) | 0/100 |
| 6 | Pd(OAc)2/XantPhos (3/6) | Cs2CO3 | THF/H2O (80) | 90/10 |
| 7 | Pd(OAc)2/(S)-BINAP (3/6) | Cs2CO3 | THF/H2O (80) | 0/100 |
| 8 | Pd(OAc)2/n-BuPAd2 (3/6) | Cs2CO3 | Toluene/H2O (100) | 100/0 |
Ratio of product/starting material as determined by GC-MS assay.
