Water → HCID 67087626, compound

Participants

Reaction Steps

0.65 g of 3-(4-dibenzothiophenyl)phenol obtained in Synthesis Example 5-(i) is placed and dissolved in 20 mL of methylene chloride; after ice cooling the flask, 0.28 g of triethylamine is added; 0.29 g of methacryloyl chloride is then added dropwise; after adding the whole, the temperature is returned to room temperature; and the mixture is stirred for 30 minutes. 10 mL of water is added; the mixture is vigorously stirred; an aqueous layer is then removed; the aqueous layer is washed with methylene chloride and then gathered with the original methylene chloride solution; and the mixture is dried upon application of magnesium sulfate. The resulting mixture is concentrated by filtration with a filter paper; and the concentrate is separated by a silica gel column (eluate: hexane/ethyl acetate=80/10 (volume ratio)) to concentrate a component having an Rf of 0.50, thereby obtaining 0.63 g (yield: 78%) of the foregoing white solid. 1H NMR (CDCl3, 400 MHz): δ (ppm) 2.09 (s, 3H), 5.77 (dd=1.6 Hz, 1H), 6.39 (s, 1H), 7.21 (m, 1H), 7.45 to 7.55 (m, 6H), 7.62 to 7.64 (m, 1H), 7.82 to 7.85 (m, 1H), 8.14 to 8.19 (m, 2H)

Provenance & Evidence