Dichloromethane → HCID 58231729, compound

Participants

Reaction Steps

1.96 g of the thus obtained 2,4-bis(3-benzothiophenyl)phenol is placed in a round bottom flask; 10 mL of methylene chloride is added to form a transparent solution; after ice cooling the flask, 0.66 g of triethylamine is added; 0.59 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 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=90/10 (volume ratio)) to concentrate a component having an Rf of 0.20, thereby obtaining 1.43 g (yield: 63%) of the foregoing white solid. 1H NMR (CDCl3, 400 MHz): δ (ppm) 5.78 (dd=1.2 & 10.8 Hz, 1H), 6.01 (dd=10.8 & 17.2 Hz, 1H), 6.26 (dd=1.2 & 17.2 Hz, 1H), 7.38 to 7.47 (m, 7H), 7.65 to 7.75 (m, 3H), 7.88 to 7.96 (m, 3H)

Provenance & Evidence