Table 5 Optimization of reaction conditions in the oxidation of 1,4-DHPs.
Entry | Solvent | Time (min) | Amount of catalyst (mg) | Temperature | Yielda (%) |
|---|---|---|---|---|---|
1 | Dichloromethane | 1080 | 117 | Reflux | 0 |
2 | Chloroform | 1080 | 117 | Reflux | 0 |
3 | Ethanol | 1080 | 117 | Reflux | 0 |
4 | Water | 1080 | 117 | Reflux | 0 |
5 | Acetonitrile | 1080 | 117 | Reflux | 0 |
6 | Formic acid | 1080 | 117 | Reflux | 0 |
7 | Tetrahydrofuran | 1080 | 117 | Reflux | 0 |
8 | Acetic acid | 10 | 117 | Reflux | 96 |
9 | Acetic acid | 120 | 117 | r. t | 85 |
10 | Acetic acid | 10 | 117 | Reflux | 96b |
11 | Acetic acid | 10 | 117 | Reflux | 96c |
12 | Acetic acid | 60 | 58 | Reflux | 73 |
13 | Acetic acid | 60 | 88 | Reflux | 85 |
14 | Acetic acid | 60 | 116 | Reflux | 90 |
15 | Acetic acid | 10 | 120 | Reflux | 96 |
16 | Acetic acid | 10 | 180 | Reflux | 96 |