Table 1.
Base | Conditiona | Temp (°C) |
Time (mins) |
Yield b (%) |
---|---|---|---|---|
- | No solvent | 90 | 15 | Trace |
- | Ethanol | 90 | 15 | Trace |
Piper idene |
Ethanol | 90 | 15 | 80 |
TMP | Ethanol | 90 | 15 | 96 |
TMP | No solvent | 90 | 15 | Trace |
DBU / pyrid ine |
Ethanol | 90 | 20 | 20 |
TMP | Acetonitrile | 90 | 15 | 76 |
TMP | Acetonitrile | 130 | 15 | 15 |
DBU | Acetonitrile | 90 | 30 | Trace |
TMP | DMF | 90 | 15 | 45 |
DMF | 90 | 30 | 10 | |
NMP | ||||
DBU | DMF | 120- 140 |
15 | Trace |
TMP | Water | 90 | 15 | Trace |
TMP | Water | 130 | 15 | Trace |
- | Water | 130 | 30 | Trace |
TMP | Toluene | 90 | 15 | Trace |
TMP | Isopropanol | 90 | 15 | 45 |
TMP | THF | 90 | 15 | 38 |
TMP | n-Butanol | 90 | 15 | 33 |
All the reaction was carried out in equimolar amount of each compound in 2 ml of solvent at 150 psi pressure.
Isolated yield