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Optimization of peracetylation using imidazole at 70 °C.
| Entry | Imidazole (Equiv.) | Reaction time (min) | Yield (% of 3) |
|---|---|---|---|
| 1 | 0.6 | 240 | 5* |
| 2 | 1.0 | 240 | 20* |
| 3 | 2.0 | 240 | 40* |
| 4 | 5.0 | 120 | 100** |
Reactions were carried out using 25 equiv Ac2O, 70°C, in DMF.
Yields estimated using TLC and ESI-MS, major products were partially acetylated compounds
confirmed by TLC, ESI-MS, and 1H NMR.
