Table 1. Optimization of solvent and Fe3O4@BTC NCs loading in the synthesis of in dihydropyrano[2,3-c]pyrazoles derivativesa.
| Entry | Catalyst (g) | Solvent | Condition | Time (min) | Yieldb (%) |
|---|---|---|---|---|---|
| 1 | Without catalyst | — | RT | 10 | Trace |
| 2 | Without catalyst | — | Reflux | 10 | 25 |
| 3 | Without catalyst | — | U.S.(60 W) (RT) | 10 | 30 |
| 4 | Fe3O4@BTC (0.01) | — | U.S.(60 W) (RT) | 10 | 50 |
| 5 | Fe3O4@BTC (0.02) | — | U.S.(60 W) (RT) | 10 | 75 |
| 6 | Fe3O4@BTC (0.03) | — | U.S.(60 W) (RT) | 10 | 80 |
| 7 | Fe3O4@BTC (0.04) | — | U.S.(60 W) (RT) | 10 | 92 |
| 8 | Fe3O4@BTC (0.05) | — | U.S.(60 W) (RT) | 10 | 92 |
| 9 | Fe3O4@BTC (0.04) | H2O | U.S.(60 W) (RT) | 20 | 30 |
| 10 | Fe3O4@BTC (0.04) | DCM | U.S.(60 W) (RT) | 10 | 40 |
| 11 | Fe3O4@BTC (0.04) | CH3OH | U.S.(60 W) (RT) | 15 | 41 |
| 12 | Fe3O4@BTC (0.04) | C2H5OH | U.S.(60 W) (RT) | 7 | 45 |
| 13 | Fe3O4 (0.04) | — | U.S.(60 W) (RT) | 15 | 35 |
| 14 | FeCl2 (0.04) | — | U.S.(60 W) (RT) | 20 | 30 |
| 15 | BTC (0.04) | — | U.S.(60 W) (RT) | 14 | 37 |
RT – room temperature; reaction conditions: benzaldehyde (1 mmol), hydrazine hydrate (1 mmol), ethyl acetoacetate (1 mmol), malononitrile (1 mmol), ultra-sonication (60 W).
Isolated yield.