Results of the selective synthesis of 1,4-PeD from FFald using bulk Ni3Sn2 pH = 8 alloy catalysts synthesised at different conditionsa.
| Entry | Catalystb | Conv.c (%) | Yieldc (%) | |||||||
|---|---|---|---|---|---|---|---|---|---|---|
| 1,4-PeD | 1,2-PeD | 1,5-PeD | FFalc | THFalc | 2H2MeTHF | 2-MeTHF | Othersd | |||
| 1 | Ni3Sn2 (2-Me-EtOH; pH = 8; 24 h; 673 K/H2) | 100 | 87 | 2 | 3 | 0 | 0 | 7 | 1 | 0 |
| 2 | Ni3Sn2 (EG; pH = 8; 24 h; 673 K/H2) | 100 | 82 | 1 | 0 | 0 | 0 | 16 | 1 | 0 |
| 3 | Ni3Sn2 (G; pH = 8; 24 h; 673 K/H2) | 100 | 81 | 3 | 2 | 0 | 0 | 11 | 3 | 0 |
| 4 | Ni3Sn2 (without polyol; pH = 8; 673 K/H2) | 100 | 14 | 16 | 12 | 0 | 22 | 36 | 0 | 0 |
| 5e | Ni3Sn2 (HT 473 K; pH = 8; 673 K/H2) | 100 | 15 | 0 | 1 | 0 | 2 | 35 | 12 | 36 |
| 6e | Ni3Sn2 (HT 523 K; pH = 8; 673 K/H2) | 100 | 3 | 5 | 3 | 0 | 7 | 22 | 0 | 61 |
| 7f | Ni3Sn2 (2-Me-EtOH; pH = 8; 24 h; 673 K/H2) | 100 | 79 | 1 | 2 | 0 | 0 | 11 | 0 | 10 |
| 8 g | Ni 3 Sn 2 (2-Me-EtOH; pH = 8; 24 h; 673 K/H 2 ) | 100 | 83 | 0 | 5 | 0 | 0 | 12 | 0 | 0 |
a
Reaction conditions: catalyst, 44 mg; substrate, 1.2 mmol; solvent, ethanol/H2O, 3.5 ml (1.5 : 2.0 volume ratio); initial H2 pressure, 3.0 MPa, 433 K, 12 h.
b
The bulk Ni3Sn2 catalysts were synthesized at various conditions.
c
Conversion of FFald and yield of the product were determined by GC and GC-MS analyses using an internal standard technique.
d
Unknown product may be the condensation product of FFald or FFalc according to GC and GC-MS data.
e
HT = hydrothermal at 473 K and 523 K.
f
The catalyst was stored in a sample bin under exposure to the air for 2 months.
g
Recyclability test after the fourth reaction run in the batch reactor system. The recovered catalyst was reactivated by H2 at 673 K for 1 h before reuse for the next run.