反应详情

Pentachlorocyclopropane (25 g, 0.116 mol) is added to a suspension of potassium hydroxide (7.8 g, 0.139 mol) in 1,4-dioxane (900 ml) and the mixture is stirred at room temperature for 30 minutes and then heated to 65° C. for a further 30 minutes. 2-Ethoxymethylfuran (17.5 g, 0.139 mol) is added to the reaction mixture, the temperature is raised to 85-90° C. and the mixture is stirred for 16 hours. The reaction mixture is cooled to room temperature, filtered through a plug of diatomaceous earth and the filtrate is evaporated under reduced pressure to give (1S*,5S*)-2,3,4,4-tetrachloro-1-ethoxymethyl-8-oxabicyclo[3.2.1]octa-2,6-diene (23 g), used without further purification in the next step.

1. temperatureheated to 65° C. for a further 30 minutes
2. temperaturethe temperature is raised to 85-90° C.
3. stirringthe mixture is stirred for 16 hours
4. temperatureThe reaction mixture is cooled to room temperature
5. filtrationfiltered through a plug of diatomaceous earth
6. customthe filtrate is evaporated under reduced pressure