Table 2 Optimization for the synthesis of pyrimidine-5-carbonitrile with 4-chlorobenzaldehyde, urea, malononitrile and bone char-nPrN-SO3H as catalyst.
Entry | Catalyst (mol%) | Solvent | Temperature (°C) | Time (min) | Yield% |
|---|---|---|---|---|---|
1 | 0.00 | - | 80 | 240 | 40 |
2 | 0.24 | - | 80 | 65 | 92 |
3 | 0.32 | - | 80 | 40 | 95 |
4 | 0.4 | - | 80 | 5 | 97 |
5 | 0.4 | Water | Reflux | 240 | 75 |
6 | 0.4 | Acetonitrile | Reflux | 240 | 50 |
7 | 0.4 | n-hexane | Reflux | 240 | 35 |
8 | 0.4 | Ethanol | Reflux | 240 | 67 |
9 | 0.4 | Ethanol: water 50:50 | Reflux | 240 | 71 |
10 | 0.4 | - | 30 | 60 | 45 |
11 | 0.4 | - | 50 | 35 | 67 |
12 | 0.4 | - | 70 | 15 | 85 |