Table 2.
Optimization of hydrolysis conditions
| |||||
|---|---|---|---|---|---|
| entry | solvent | acid (equiv) | T (°C) | t (h) | yielda |
| 1 | EtOH | 1M aq H2SO4 (6) | rt | 8 | NR |
| 2 | MeOH | H2SO4 (6) | reflux | 1 | 8 % |
| 3 | MeOH | 50% aq H2SO4 (6) | reflux | 0.16 | 84 % |
| 4 | MeOH | 50% aq H2SO4 (6) | rt | 48 | 19 % |
| 5 | MeOH | 30% aq H2SO4 (6) | rt | 1.5 | NR |
| 6 | THF | camphorsulfonic (2) | rt | 3 | NR |
| 7 | THF | 50% aq H2SO4 (6) | 55 | 3 | 78 % |
| 8 | THF | 50% aq H2SO4 (6) | rt | 24 | 20 % |
Isolated yields. Cyclododecanone recovered in comparable yields.