Table 4.
Rhodium-catalyzed reductive carbonylation of iodobenzene with CO and H2 to afford benzaldehyde: effects of dosage of RhCl3·3H2O and PPh3a.
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Entry | RhCl3·3H2O [mol %] |
PPh3 [mol %] |
Conversion [%]b |
Yield [%]b |
1 | 1 | 2 | 35 | 28 |
2 | 1 | 3 | 51 | 47 |
3 | 1 | 4 | 78 | 74 |
4 | 1 | 5 | 72 | 70 |
5 | 2 | 4 | 34 | 31 |
6 | 2 | 6 | 65 | 62 |
7 | 2 | 8 | 92 | 88 |
8 | 2 | 10 | 88 | 84 |
9 | 2.5 | 5 | 47 | 42 |
10 | 2.5 | 7.5 | 81 | 73 |
11 | 2.5 | 10 | 100 | 97 |
12 | 2.5 | 12.5 | 100 | 92 |
13 | 3 | 12 | 100 | 97 |
14 | 4 | 16 | 100 | 97 |
15 | 5 | 20 | 100 | 97 |
aStandard conditions: PhI (1 mmol), RhCl3·3H2O, PPh3, Et3N (1.2 mmol), DMA (2 mL), CO/H2 (5 bar:5 bar), 90 °C, 12 h. bDetermined by GC using dodecane as an internal standard.