Table 1.
Effect of various amounts of catalysts, temperature and solvents in synthesis of pyrazolo[4′,3′:5,6]pyrido[2,3-d]pyrimidines.
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Entry | Solvent | Catalyst (mg) | Temp. (˚C) | Time (min.) | Yield (%) |
1 | – | 5 | 100 | 40 | 70 |
2 | – | 10 | 100 | 15 | 91 |
3 | – | 20 | 100 | 35 | 72 |
4 | – | – | 100 | 120 | - |
5 | – | 10 | 110 | 20 | 85 |
6 | – | 10 | 50 | 60 | 46 |
7 | – | 10 | 25 | 70 | 40 |
8 | EtOH | 10 | Reflux | 45 | 70 |
9 | DMF | 10 | 100 | 100 | 30 |
10 | H2O | 10 | Reflux | 120 | – |
11 | CH3CN | 10 | Reflux | 120 | Trace |
12 | n-Hexane | 10 | Reflux | 120 | – |
13 | CHCl3 | 10 | Reflux | 100 | 35 |
14 | Toluene | 10 | Reflux | 120 | – |
15 | MeOH | 10 | Reflux | 60 | 60 |
16 | CH2Cl2 | 10 | Reflux | 65 | 35 |
17 | EtOAc | 10 | Reflux | 120 | – |