Table 2.
Optimization and scope for flow application
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|---|---|---|
| Entry | Deviations from standard conditionsa | Yieldb |
| 1 | None | 85% |
| 2 | DMF/ACN 3:1, 60W | 78% |
| 3 | DMF, NaHSO4 (1 equiv) | traces |
| 4 | 45°C | 49% |
| 5 | Catalyst loading = 2.5 mol% | 71% |
| 6c | In batch under blue-lights (2 × 40W) | traces |
| 7 | Stop-flow | 37% |
Scope:
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Reaction conditions: solution A: 1a (0.2 mmol), 3a (0.6 mmol) and iridium photocatalyst (3.5 mol%) in DMF/ACN (2 mL). Solution B: 2a (0.3 mmol) in DMF/ACN (2 mL). Solution A and B were pumped at 0.1 mL/min.
The yields were based on isolated products.
No stirring.
