Effects of various factors on the synthesis of 4aa.
| |||||
|---|---|---|---|---|---|
| Entry | Nanocatalyst (g) | Conditions | Solvent (3 mL) | Time (min) | Yieldb (%) |
| 1 | — | Grinding, r.t. | — | 30 | Trace |
| 2 | — | 80 °C | — | 180 | Trace |
| 3 | 0.005 | Grinding, r.t. | — | 30 | 25 |
| 4 | 0.007 | Grinding, r.t. | — | 30 | 32 |
| 5 | 0.01 | Grinding, r.t. | — | 20 | 37 |
| 6 | 0.03 | Grinding, r.t. | — | 20 | 45 |
| 7 | 0.05 | Grinding, r.t. | — | 20 | 91 |
| 8 | 0.07 | Grinding, r.t. | — | 15 | 95 |
| 9 | 0.09 | Grinding, r.t. | — | 15 | 90 |
| 10 | 0.1 | Grinding, r.t. | — | 15 | 88 |
| 11 | 0.07 | Reflux | EtOH | 4 h | 55 |
| 12 | 0.07 | Reflux | EtOH/H2O (1 : 1) | 3 h | 60 |
| 13 | 0.07 | Reflux | H2O | 7 h | 20 |
| 14 | 0.07 | Reflux | Toluene | 5 h | 30 |
| 15 | 0.07 | Reflux | Chloroform | 5 h | 12 |
Reaction conditions: benzaldehyde (1 mmol), dimedone (1 mmol), malononitrile (1 mmol), catalysts, under different conditions.
Isolated pure yield.