Magnesium Chloride → HCID 14795414, compound

Participants

Reaction Steps

A mixture of 4.4 grams (0.011 mole) of 4-(trifluoromethylsulfonyloxy)-4'-(2-methyl-2-propenoxy)benzophenone and 0.05 gram (0.0005 mole) of magnesium chloride was stirred under a nitrogen atmosphere at 170°-175° C. for 20 hours. The reaction mixture was cooled to ambient temperature, and diethyl ether was added. The mixture was filtered through diatomaceous earth, and the filtrate was placed in a separatory funnel and washed with two portions of aqueous 0.5 N sodium hydroxide, three portions of water, and one portion of a saturated, aqueous, sodium chloride solution. The organic layer was dried with sodium sulfate and filtered. The filtrate was concentrated under reduced pressure to a residue. The residue was purified by centrifically accelerated, radial thin layer chromatography. Elution was accomplished using 3:1 methylene chloride:hexane. The appropriate fractions were combined and concentrated under reduced pressure to yield 1.7 grams of (4-trifluoromethylsulfonyloxyphenyl)(2,3-dihydro-2,2-dimethylbenzofuran-5-yl) ketone. The nmr spectrum was consistent with the proposed structure.

Provenance & Evidence