Dichloromethane → HCID 58231717, compound

Participants

Reaction Steps

1.02 g of the thus obtained 2,4-bis(4-dibenzothiophenyl)phenol is placed in a round bottom flask; 5 mL of methylene chloride is added to form a transparent solution; after ice cooling the flask, 0.27 g of triethylamine is added; 0.24 g of acryloyl 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=80/20 (volume ratio)) to concentrate a component having an Rf of 0.42, thereby obtaining 1.0 g (yield: 88%) of the foregoing white solid. 1H NMR (CDCl3, 400 MHz): δ (ppm) 6.05 (dd=1.2 & 10.4 Hz, 1H), 6.37 (dd=10.4 & 17.2 Hz, 1H), 6.66 (dd=1.2 & 17.2 Hz, 1H), 7.30 to 8.25 (m, 17H)

Provenance & Evidence