Table 2.
Optimization of acylation conditions.
| |||||
|---|---|---|---|---|---|
| Entry | Base | Solvent | temp (°C) | conc. (M) | Yield (%) |
| 1 | NaOt-Bu | DME | rt | 0.1 | 27 |
| 2 | NaH | DME | rt | 0.1 | 74 |
| 3 | KOt-Bu | DME | rt | 0.1 | 63 |
| 4 | n-BuLi | THF | –78 | 0.1 | n.d. |
| 5 | n-BuLi | THF | 0 | 0.1 | n.d. |
| 6 | i-PrMgCl | THF | 0 | 0.1 | 90a |
| 7 | i-PrMgCl | THF | 0 | 0.2 | 74 |
DME = 1,2-dimethoxyethane