Table 2. Catalytic CO2 Hydrogenation with 1 Using Different H2/CO2 Partial Pressure Ratiosa.
| entry | 1/DBU | pH2/pCO2 (bar) | TONb | yield (%)c |
|---|---|---|---|---|
| 1 | 1/1000 | 50/25 | 1000 | 100 |
| 2 | 1/1000 | 60/20 | 1000 | 100 |
| 3 | 1/2000 | 50/25 | 540 | 26.8 |
| 4 | 1/5000 | 50/25 | 98 | 1.9 |
| 5 | 1/10 000 | 50/25 | 109 | 1.1 |
Reaction conditions: catalyst 1, 1–10 μmol; DBU, 10 mmol; THF, 5.5 mL; H2/CO2 (2:1 or 3:1) pressure; 80 °C, 24 h.
TON = (mmol formate)/(mmol catalyst).
Yield = [(mmol formate)/(mmol DBU)] × 100. The amount of formate was calculated from the integration of the corresponding 1H NMR signal in D2O against an internal standard (DMF). All experiments were repeated at least twice to check for reproducibility; average error, ca. 6%.