Effect of different amounts of catalysts, temperature and solvent (5 mL) in the synthesis of picolinate and picolinic acid derivatives.
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Entry | Catalyst (mg) | Solvent | Temperature (°C) | Time (min) | Yield (%) |
1 | 5 | DMF | 100 | 60 | 80 |
2 | 5 | H2O | Reflux | 120 | 25 |
3 | 5 | n-Hexane | Reflux | 120 | — |
4 | 5 | CH3CN | Reflux | 120 | 60 |
5 | 5 | CHCl3 | Reflux | 180 | 50 |
6 | 5 | CH2Cl2 | Reflux | 150 | — |
7 | 5 | EtOAc | Reflux | 180 | — |
8 | 5 | MeOH | Reflux | 180 | 45 |
9 | 5 | EtOH | Reflux | 100 | 60 |
10 | 5 | EtOH | 50 | 80 | 72 |
11 | 5 | EtOH | 25 | 60 | 88 |
12 | 2.5 | EtOH | 25 | 80 | 70 |
13 | 10 | EtOH | 25 | 60 | 88 |
14 | — | EtOH | 25 | 60 | Trace |
15 | 5 | — | 25 | 180 | — |
16 | 5 | — | 100 | 100 | 25 |