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Survey of Dipolarophiles and Reaction Conditions 
| Entry | Alkyne | Solvent | Temp. (time) | Conv. (%) |
|---|---|---|---|---|
| 1 | DPA | CH3CN | reflux (26h) | 0 |
| 2 | DPA | EtOH | reflux (32h) | 0 |
| 3 | PA | CH3CN | reflux (24h) | 0 |
| 4 | DMAD | MeOH | reflux (4 h) | 93a |
| 5 | DMAD | D2O | r.t. (12 h) | 50a |
| 6 | DMAD | D2O | 70 °C (3 h) | >99 |
| 7b | DEBD | EtOH | 30 °C (96 h) | 86a |
| 8 | DEBD | EtOH | reflux (10h) | >99 |
| 9 | DEBD | CDCl3 | reflux (32h) | >99 |
| 10 | DEBD | CH3CN | reflux (4 h) | >99 |
By‐products detected in NMR.
Cu wire catalyst added.
