Table 2.
entry | allenamidesa | time [h] | cycloadducts | yield [%]b |
---|---|---|---|---|
1 | 13a: R = p-Ns | 12 | 14a: R = p-Ns | 92 |
2 | 13b: R = Boc | 20 | 14b: R = Boc | 65 |
3 | 13c: R = (−)-menthyl | 20 | 14c: R = (−)-menthyl | 54c |
4 | (±)-15a: R = Ph | 2 | 16a: R = Ph | 77d |
5 | (±)-15b: R = Me | 30 | 16b: R = Me | 57d |
6 | 17 | <12 | 19 | 77 |
7 | 18 | 4 | 20 | 93 |
8 | 21 | 24 | 23 | 95e |
9 | 24 | 20 | 25 | 78 |
Unless otherwise noted, all reactions were carried out in THF at 85 °C at concn = 0.10 M. Reactions in entries 3 and 8 were run in toluene. Entries 4 and 8 were run at 45 °C and 110 °C, respectively.
Isolated yields.
Only one isomer by 1H NMR but absolute configuration unassigned.
16a and 16b were found as a ~ 3:1 inseparable isomeric mixture.
Regioisomeric ratio of regioisomers 22 and 23 is ~ 4:1.