Table 3 Comparative performances of the Talc catalyst for the synthesis of dihydropyranochromene in different conditions.
Entry | Condition solvent/catalyst (g) | Condition | Time (min) | Yield (%)a |
|---|---|---|---|---|
1 | –/Talc (0.04) | Mixer Mil 10 Hz | 20 | Trace |
2 | –/Talc (0.04) | Mixer Mil 15 Hz | 20 | Trace |
3 | –/Talc (0.04) | Mixer Mil 20 Hz | 20 | Trace |
4 | –/Talc (0.06) | Mixer Mil 20 Hz | 20 | Trace |
5 | –/- | Reflux | 90 | Trace |
6 | H2O/- | Reflux | 90 | Trace |
7 | C2H5OH/- | Reflux | 90 | 10 |
8 | C2H5OH/Talc (0.01) | Reflux | 90 | 43 |
9 | C2H5OH/Talc (0.02) | Reflux | 90 | 61 |
10 | C2H5OH/Talc (0.04) | Reflux | 90 | 78 |
11 | C2H5OH/Talc (0.06) | Reflux | 90 | 95 |
12 | C2H5OH: H2O/Talc (0.04) | R.T. | 120 | 57 |
13 | C2H5OH/NaOH (0.04) | Reflux | 20 | 50b |
14 | C2H5OH/K2CO3 (0.04) | Reflux | 180 | 95b |
15 | C2H5OH/MgO (0.04) | Reflux | 120 | 98b |
16 | C2H5OH/Hydrotalcite (0.04) | Reflux | 150 | 95b |