Table 1.
Optimization of the reaction conditions.
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| Entry | Rh cat. | Solvent | Time (h) | Yielda | dr [syn:anti]b,c |
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| 1 | RhCl(PPh3)3 | THF | 1 | 64 | [3:1] |
| 2 | [RhCl(cod)]2 | THF | 1.5 | 72 | [30:1] |
| 3 | RhClCO(PPh3)2 | THF | 1 | 85 | [9:1] |
| 4 | Rh(acac)(CO)2 | THF | 1 | trace | – |
| 5 | [RhCl(cod)]2 | toluene | 1 | 68 | [14:1] |
| 6 | [RhCl(cod)]2 | AcOEt | 1 | 79 | [25:1] |
| 7 | [RhCl(cod)]2 | CH2Cl2 | 1 | 77 | [31:1] |
| 8 | [RhCl(cod)]2 | DME | 2 | 17d | – |
| 9 | [RhCl(cod)]2 | CH3CN | 1 | 71 | [2:1] |
| 10 | [RhCl(cod)]2 | DMF | 3 | 42 | [1:27] |
| 11 | [RhCl(cod)]2 | DMPU | 1 | 52 | [1:50] |
aIsolated yield; bthe stereochemistry between CH3 (Cα) and OH (Cβ) moieties; cdiastereomeric ratio was determined after purification; ddiastereomeric mixture.