Table 1. Solvent Screening for the Synthesis of 8aa.
| entry | solvent | time (h) | yieldb (%) |
|---|---|---|---|
| 1 | CH3CN | 24 | n.r. |
| 2 | IPA | 24 | 27 |
| 3 | DMF | 24 | n.r. |
| 4 | EtOH | 24 | 70 |
| 5 | THF | 24 | n.r. |
| 6 | DCM | 24 | n.r. |
| 7 | CHCl3 | 24 | n.r. |
| 8 | H2O | 24 | 39 |
| 9 | MeOH | 24 | 61 |
| 10 | solvent-free | 24 | 25 |
| 11c | neat | 12 | 46 |
| 12 | EtOH:H2O (1:1 v/v: 5 mL) | 5.5 | 78 |
| 13 | EtOH:H2O (1:1 v/v: 10 mL) | 2.5 | 93 |
| 14 | EtOH:H2O (1:2 v/v: 10 mL) | 5 | 75 |
| 15 | EtOH:H2O (2:1 v/v: 10 mL) | 7 | 69 |
Reaction conditions: 5 (1 equiv), 6a (1 equiv), and 7 (1 equiv) at room temperature. 5 mol % catalyst.
Yield of the isolated product.
60 °C. n.r.—no reaction
