Table 1.
| |||
---|---|---|---|
entry | conditions* | dr† | yield (%)‡ |
1 | Co2(CO)8 (1.2 equiv), THF, 12 h; then DMSO, 65 °C | 2.2 : 1 | 46 |
2 | Co2(CO)8 (1.2 equiv), CH2Cl2, 9 h; then NMO, 23 °C | 4.5 : 1 | 78 |
3 | Mo(CO)6 (1.2 equiv), DMSO, PhMe, 110 °C | -- | trace |
4 | Mo(CO)3(DMF)3 (1.1 equiv), CH2Cl2, 23 °C | > 20 : 1 | 67 |
5 | [RhCl(CO)2]2 (1 mol %), CO (1 atm), m-xylene, 110 °C | >20 : 1 | 85 |
Reactions conducted on 0.2 mmol scale.
Determined by 1H NMR spectroscopy.
Isolated yield after purification by silica gel chromatography.