Dichloromethane → HCID 58231738, compound

Participants

Reaction Steps

1.35 g of the thus obtained 2,6-bis(4-dibenzothiophenyl)-4-methylphenol is placed in a round bottom flask; 20 mL of methylene chloride is added; after ice cooling the flask, 0.33 g of triethylamine is added; 0.30 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 0.85 g (yield: 57%) of the foregoing white solid. 1H NMR (CDCl3, 400 MHz): δ (ppm) 2.57 (s, 3H), 5.41 (dd=1.2 & 10.4 Hz, 1H), 5.64 (dd=10.4 & 17.2 Hz, 1H), 5.97 (dd=1.2 & 17.2 Hz, 1H), 7.49 to 7.59 (m, 10H), 7.90 (m, 2H), 8.16 to 8.21 (m, 4H)

Provenance & Evidence