反应详情

To a suspension of sodium hydride (80%, 3.3 g, 0.11 mol) in dry toluene (250 ml) under argon, was added dropwise a solution of δ-valerolactam (9.9 g, 0.10 mol) in toluene (50 ml). When the addition was complete, the mixture was heated under reflux for 1 h, then cooled to ambient temperature. A solution of benzyl bromide (13 ml, 18.8 g, 0.11 mol) in toluene (50 ml) containing dimethyl formamide (1 ml) was then added dropwise over 15 minutes. The resulting mixture was heated under reflux for 4 h. On cooling, the mixture was filtered and the filtrate was dried (Na2SO4) and evaporated in vacuo to give an oil. Bulb-to-bulb distillation gave the title compound (D26) as a yellow oil (8.0 g).

1. additionWhen the addition
2. temperaturethe mixture was heated
3. temperatureunder reflux for 1 h
4. additionwas then added dropwise over 15 minutes
5. temperatureThe resulting mixture was heated
6. temperatureunder reflux for 4 h
7. temperatureOn cooling
8. filtrationthe mixture was filtered
9. dry with materialthe filtrate was dried (Na2SO4)
10. customevaporated in vacuo
11. customto give an oil
12. distillationBulb-to-bulb distillation