Table 1.
entry | (2/3/1) | solvent | T (°C), t (h) | yield (%)b |
---|---|---|---|---|
1 | 1/2/2 | THF | 0, 30 | 44 |
2 | 1/2/2 | Et2O/THF (20/1) | 0, 30 | 29 |
3 | 1/2/2 | Et2O | 0, 30 | 48 |
4 | 1/2.5/2 | Et2O | 0, 30 | 40 |
5 | 1/1.5/2 | Et2O | 0, 30 | 41 |
6 | 1/2/3 | Et2O | 0, 30 | 67 |
7 | 1/2/3 | Et2O | 25, 30 | 61 |
8 | 1/2/3 | Et2O | −78, 30 | trace |
Aryne precursor (0.25 mmol), solvent (1.5 mL).
Yields determined by GC analysis with n-decane as an internal standard.