反应详情

To a refluxing suspension of copper powder (5.0 g, 0.079 mole) in 240 ml of n-octane was added dropwise in one hour a solution of ethyl (±)-3-methyl-1-trichloromethyl-2-butenyl diazomalonate (5.0 g, 0.0146 mole) in 60 ml of n-octane. The reaction mixture was then heated under reflux for 21/2 hours and filtered. The n-octane was removed from the filtrate by evaporation under vacuum, yielding a residue which was distilled under vacuum to give ethyl (±)-4-trichloromethyl-6,6-dimethyl-2-oxo-3-oxabicyclo-[3.1.0]hexane-1-carboxylate as a highly viscous oil (2.47 g, 54% yield); bp, 123°-125°/0.3 mm.

1. temperatureThe reaction mixture was then heated
2. temperatureunder reflux for 21/2 hours
3. filtrationfiltered
4. customThe n-octane was removed from the filtrate by evaporation under vacuum
5. customyielding a residue which
6. distillationwas distilled under vacuum