Optimization of the reaction conditions for the synthesis of biscoumarin derivatives catalyzed by P4VPy.
| Entry | Catalyst (mg) | Solvent | Temperature (°C) | Time (min) | Yield (%) |
|---|---|---|---|---|---|
| 1 | — | No solvent | RT | 120 | Nil |
| 2 | — | No solvent | 100 | 120 | Nil |
| 3 | 20 | CH3CN | RT | 120 | Nil |
| 4 | 20 | CH3CN | Reflux | 120 | Mixture of products |
| 5 | 20 | CH2Cl2 | RT | 120 | Nil |
| 6 | 20 | CH2Cl2 | Reflux | 120 | Mixture of products |
| 7 | 20 | EtOH | RT | 120 | 30 |
| 8 | 20 | EtOH | Reflux | 120 | 60 |
| 9 | 10 | H2O | RT | 90 | 40 |
| 10 | 15 | H2O | RT | 90 | 50 |
| 11 | 20 | H2O | RT | 90 | 75 |
| 12 | 20 | H2O | 90 | 5 | 96 |
| 13 | 24 | H2O/EtOH | 90 | 5 | 96 |