Optimization of reaction conditionsa.
| ||
|---|---|---|
| Entrya | Variation from standard conditions | Yieldb |
| 1 | None | 99%c (97%) |
| 2 | Mn instead of Zn | n.o. |
| 3 | Fe instead of Zn | n.o. |
| 4 | Toluene instead of MeCN | <5% |
| 5 | No catalyst | n.o. |
| 6 | No ligand | Trace |
| 7 | Pd(TFA)2 instead of Pd(OAc)2 | 94% |
| 8 | Xantphos instead of DPPP | 31% |
| 9 | Ni(acac)2 + L1 as catalyst | n.o. |
| 10 | CuI + L1 as catalyst | n.o. |
| 11 | 1 bar CO | 91% |
Reaction conditions: 1a (0.2 mmol), 2a (0.3 mmol), CO (10 bar), Pd(OAc)2 (1 mol%), DPPP (1 mol%), Zn (0.3 mmol) in MeCN (2 mL) at 80 °C for 20 h.
Yields were determined by GC-FID analysis using n-dodecane as the internal standard.
Yield of the isolated product. n.o. = not observed.