Table 8. Influence of the Reused 10% Pd/C Catalyst on the Ratio of Byproducts in the Hydrogenation of PPNa.
| composition
of byproduct |
|||||||
|---|---|---|---|---|---|---|---|
| no. | reusing the catalyst | purity of PPA (%) | PPN (%) | TPPA (%) | BPPA (%) | PPAL (%) | PPOH (%) |
| 1 | -(fresh) | 99.0 | 29.9 | 68.3 | 0 | 1.3 | 0.5 |
| 2 | 1st | 69.6 | 66.0 | 26.3 | 0 | 7.6 | 0.1 |
| 3 | -(fresh)b | 99.8 | 33.5 | 64.6 | 0 | 1.3 | 0.6 |
| 4 | 1stb | 99.7 | 32.5 | 65.8 | 0 | 1.2 | 0.5 |
Conditions: 5.0 g (38.2 mmol) PPN, 1.5 g 10% Pd/C (Selcat Q) catalyst, 250 mL of water and 50 mL dichloromethane, 5.27 g NaH2PO4·H2O (38.2 mmol), and 3.82 g conc. H2SO4 (38.2 mmol), 80 °C, 6 bar, reaction time: 7 h.
10% Pd/C catalyst was prehydrogenated in 200 mL water, at 30 °C and 6 bar, for 0.5 h.