Hydrochloric Acid → HCID 23451898, compound

Participants

Reaction Conditions

Reaction Steps

15 g anhydrous potassium sulfide and 100 ml DMF are added into a 250 ml three-neck flask. The solution is heated to 50° C. under stirring, and then 8 g 4-chloro-4′-phenyl benzophenone is added into the solution; the solution is heated to reflux (about 110° C.), and is cooled after 7 h; adding 100 ml methylbenzene, regulating the pH value to 5-6 with diluted hydrochloric acid, and separating the solution; the organic phase is extracted twice with 50 ml NaOH solution having a content of 5%, and the aqueous phases are mixed; the obtained aqueous phase is put into a 250 ml three-neck flask, and nitrogen is supplied to blow for 30 min, then 15% hydrochloric acid is dropped into the aqueous solution while agitating to regulate the pH value to 5-6, and light yellow solid precipitate; filtering to obtain a light yellow solid, and the weight after drying at a reduced pressure is 5.0 g, the purity is 99.11%, the yield is 63%, the melting point is 173˜176.7° C., and 1H-NMR data (solvent CDCl3): δ3.654 ppm, s, 1H; δ7.432, 7.370 ppm, d, 2H; δ7.413, 7.436 ppm, d, 1H; δ7.466, 7.491, 7.515 ppm, t, 2H; δ7.641, 7.665 ppm, d, 2H; δ7.695, 7.719 ppm, 7.743, t, 4H; δ7.850, 7.874 ppm, d, 2H.

Provenance & Evidence