Table 5 Optimization of Biginelli reactiona.
From: A copper-doped ZIF-8: a high-performance catalyst for eco-friendly Ullmann and Biginelli reactions
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|---|---|---|---|---|---|---|
Entry | Solvent | T (°C) | Cat. (mg) | Yield (%) | TON | TOF(h− 1) |
1 | EtOH | Reflux | – | 0 | 0 | 0 |
2 | EtOH | Reflux | 20.0 | 80 | 307.7 | 205.1 |
3 | EtOH | Reflux | 30.0 | 90 | 230.8 | 153.8 |
4 | EtOH | Reflux | 40.0 | 83 | 159.6 | 106.4 |
5 | EtOH | Reflux | 50.0 | 78 | 120 | 80 |
6 | EtOH | Reflux | ZIF-8 (30) | trace | – | – |
7 | EtOH | Reflux | Cu(NO3)2·6H2O (30) | 27 | 69 | 46 |
8 | EtOH | Reflux | Cu(NO3)2·6H2O (30) + ZIF-8 (30) | 40 | 102.6 | 68.4 |
9 | H2O | 80 | 30.0 | 0 | 0 | 0 |
10 | EtOAc | Reflux | 30.0 | 40 | 102.6 | 68.4 |
11 | CH3CN | Reflux | 30.0 | 52 | 133.3 | 88.9 |
12 | Toluene | 80 | 30.0 | 10 | 25.6 | 17.1 |
13 | CHCl3 | Reflux | 30.0 | 25 | 64.1 | 42.7 |
14 | MeOH | Reflux | 30.0 | 59 | 151.3 | 100.9 |
15 | EtOH | r.t | 50.0 | 45 | 69.2 | 46.2 |
16 | EtOH | 60 | 50.0 | 76 | 116.9 | 77.9 |
17 | EtOH | 70 | 50.0 | 84 | 129.2 | 86.2 |
