反应详情

A stirred mixture of 1.64 grams (0.068 mole) of magnesium turnings in 200 mL of methanol was warmed to reflux, and a solution of 3.0 grams (0.0068 mole) of 1-cyclopropyl-1-(4-trifluoromethoxyphenyl)-4-(4-fluoro-3-phenoxyphenyl)-1,3-butadiene was added dropwise. Upon completion of addition the reaction mixture was heated at reflux for one hour. The reaction mixture was cooled and stirred with ethyl acetate and aqueous 3N hydrochloric acid. The mixture was filtered, the organic layer was separated from the filtrate, and it was washed in turn with aqueous 1N hydrochloric acid and water. The organic layer was dried with magnesium sulfate and filtered. The filtrate was concentrated under reduced pressure yielding 2.5 grams of 1-cyclopropyl-1-(4-trifluoromethoxyphenyl)-4-(4-fluoro-3-phenoxyphenyl)-2-butene.

1. temperaturewas warmed
2. temperatureto reflux
3. additionUpon completion of addition the reaction mixture
4. temperaturewas heated
5. temperatureat reflux for one hour
6. temperatureThe reaction mixture was cooled
7. filtrationThe mixture was filtered
8. customthe organic layer was separated from the filtrate, and it
9. washwas washed in turn with aqueous 1N hydrochloric acid and water
10. dry with materialThe organic layer was dried with magnesium sulfate
11. filtrationfiltered
12. concentrationThe filtrate was concentrated under reduced pressure