Table 1. Investigation of Reaction Conditionsa.
| entry | catalyst | solvent | T[°C] | yield 2a | yield 3a |
|---|---|---|---|---|---|
| 1 | Ru–Mo–S-0.33 | toluene | 150 | 71% | 29% |
| 2 | Ru–Mo–S-0.33 | toluene | 120 | 89% | 4% |
| 3 | Rh–Mo–S-0.33 | toluene | 120 | 39% | 1% |
| 4 | Co–Mo–S-0.33 | toluene | 120 | 79% | 2% |
| 5 | Pd–Mo–S-0.33 | toluene | 120 | 44% | 3% |
| 6 | Ru–Mo–S-0.33 | EtOH | 100 | 96% | 3% |
| 7 | Ru–Mo–S-0.33 | MeOH | 80 | 96% | 4% |
| 8 | Ru–Mo–S-0.33 | MeOH | 60 | 51% | 0% |
| 9 | Ru–Mo–S-0.50 | MeOH | 60 | 90% | 3% |
| 10 | Ru–W–S-0.33 | MeOH | 60 | 96% | 2% |
| 11 | Ru–S | MeOH | 60 | 32% | 0% |
| 12 | Ru–S–SO4 | MeOH | 60 | 76% | 0% |
a
Reaction conditions: 1a (0.1 mmol), cat. (2.2 mg), H2 (40 bar), solvent (0.66 mL), and reaction time = 24 h. Yields were determined by GC-FID using mesitylene as internal standard. [M] = metal catalyst.