Table 1.
Entry | Conditionsa | Time | Conversionb |
---|---|---|---|
1 | 1, 24 °C | 1 h | 0% |
1, 70 °C | 1 h | 0% | |
1, 70 °C | 16 h | 0% | |
2 | AgOTf, 70 °C | 1 h | 0% |
AgOTf, 70 °C | 16 h | 0% | |
3 | 1, + AgOTf, 24 °C | 1 h | 0% |
1, + AgOTf, 70 °C | 1 h | 48% | |
1, + AgOTf, 70 °C | 16 h | 99% | |
4 | 2, 70 °C | 1 h | 0% |
2, 70 °C | 16 h | 0% | |
5 | 2 + AgOTf, 24 °C | 1 h | 0% |
2 + AgOTf, 70 °C | 1 h | 7% | |
2 + AgOTf, 70 °C | 16 h | 99% | |
6 | AuCl, 70 °C | 16 h | 11% |
7 | AuCl, + AgOTf, 70 °C | 16 h | 8%c |
[12] = 0.04 mM, [Au] = 0.002 mM (5 mol%), [additive] = 0.004 mM (10 mol%), reaction volume 0.60 mL.
As determined by NMR integration, all species were cleanly resolved and except for entry 7, the only observable compounds were starting 12 or product 24.
6% of fluorene 5 was detected.