反应详情

In an argon atmosphere, the unpurified 2-diazo-3-oxo-6-heptenoic acid methyl ester of Preparation 1 (4.55 g, 25 mmol) was dissolved in 100 ml of benzene. Anhydrous cupric sulfate (2.5 g) was added as a catalyst to the solution. The mixture was stirred for about 3 hours under reflux. After confirming the disappearance of the starting materials by thin layer chromatography, the reaction mixture was filtered through a Celite column. The solvvent was distilled off from the filtrate under reduced pressure and the remaining oily product was distilled under a reduced pressure to obtain 2.92 g of 2-oxo-bicyclo[3.1.0]hexane-1-carboxylic acid methyl ester as an oily product.

1. temperatureunder reflux
2. filtrationthe reaction mixture was filtered through a Celite column
3. distillationThe solvvent was distilled off from the filtrate under reduced pressure
4. distillationthe remaining oily product was distilled under a reduced pressure