Table 1.
Optimization of ortho-halogenation reaction. X =halide.
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|---|---|---|---|---|---|
| Entry | Additive (equiv) | Hal | Solvent | T [8C] | Yield [%][a] |
| 1 | none | Br | PrCN | 80 | 50 |
| 2 | none | Br | PrCN | 100 | 65 |
| 3 | AcOH (50) | Br | PrCN | 80 | 15 |
| 4 | Cu(OAc)2 (1) | Br | PrCN | 100 | trace |
| 5 | PhI(OAc)2 (1.5) | Br | PrCN | 80 | 80 |
| 6 | PhI(OAc)2 (1.5) | Br | PrCN | 100 | 65 |
| 7 | PhI(OAc)2 (1.5) | Br | C2H4Cl2 | 60 | 85 |
| 8 | PhI(OAc)2 (1.5) | I | C2H4Cl2 | 65 | 95 |
| 9 | PhI(OAc)2 (1.5) | Cl | C2H4Cl2 | 65 | 42 |
Yield determined by NMR spectroscopy.
