Table 2.
MW-assisted nitrobenzene reduction optimization.
| Entry | Method | System | Apparatus | Reaction time (min) | Yield (%)a |
|---|---|---|---|---|---|
| 1 | MW-T constantb | Anton Paar Monowave 300 | Monomode | 15 | 21 |
| 30 | >99 | ||||
| 2 | MW-P constantc | Anton Paar Monowave 300 | Monomode | 15 | 49 |
| 30 | >99 | ||||
| 3 | MW-T constantb | CEM, Discover | Monomode | 15 | 22 |
| 30 | >99 | ||||
| 4 | MW-P constantc | CEM, Discover | Monomode | 15 | 53 |
| 30 | >99 | ||||
| 5 | MW-T constantb | CEM, MARS | Multimode | 15 | 52 |
| 30 | >99 | ||||
| 6 | MW-P constantd | CEM, MARS | Multimode | 15 | >99 |
| 30 | >99 | ||||
| 7 | MW-T constantb | Milestone, MicroSynth | Multimode | 15 | 58 |
| 30 | >99 | ||||
| 8 | MW-P constantd | Milestone, MicroSynth | Multimode | 15 | >99 |
| 30 | >99 |
Reaction conditions: CuNPs (5 mol%) and glycerol were sonicated for 10 min, creating a perfectly dispersed black solution. Nitrobenzene (1 eq) and KOH (2 eq) where then added.
a
Determined by GC-MS.
b
Program: 2 min Pmax = 400 W heated as quickly as possible to reach 130°C, then T = 130°C.
c
Program: 2 min Pmax = 100% heated as quickly as possible to reach 130°C, then P: 4 W.
d
Program: 2 min Pmax = 400 W heated as quickly as possible to reach 130°C, then P: 80 W.