Table 2.
Optimization of the reaction conditionsa
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|---|---|---|---|---|---|
| entry | solvent | additive | 2a/3ab | dr (2a)b | yield (%)c |
| 1 | CH2Cl2 | none | < 5:95 | -- | -- |
| 2 | CH2Cl2 | K2CO3 | 83:17 | 5:1 | 46 |
| 3 | Toluened | K2CO3 | complex mixture | ||
| 4 | CH3CN | K2CO3 | complex mixture | ||
| 5 | CH2Cl2 | MS 4Å | 70:30 | 10:1 | 38 |
| 6 | CH2Cl2 | Cs2CO3 | 94:6 | 2:1 | 42 |
| 7 | CH2Cl2 | MgO | 70:30 | 7:1 | 45 |
| 8e | CH2Cl2 | K2CO3 | > 95:5 | 7:1 | 62 |
Unless otherwise noted, all the reactions were performed by adding PhI(OAc)2 to a suspension of 1a, N-aminophthalimide and the additive.
Determined by 1H NMR of the crude reaction mixture.
Isolated yield.
12 h.
Allylic alcohol 1a was added the last.
