Potassium Iodide → HCID 13536203, compound

Participants

Reaction Steps

A mixture of 10 g of methyl 7-methoxy-3-oxo-3,4-dihydro-2H-1,5-benzoxathiepin-4-carboxylate, 9.8 g of 3-(4-phenylpiperazin-1-yl)propyl chloride, 6.2 g of anhydrous potassium carbonate, 3.0 g of potassium iodide and 150 ml of methyl ethyl ketone is stirred with heating under reflux for 25 hours. After the mixture is cooled, the inorganic substance is filtered off, and the filtrate is concentrated under reduced pressure. The resulting residue is dissolved in ethyl acetate, and the solution is washed with water and dried. The solvent is evaporated off under reduced pressure, and the resulting residue is purified by column chromatography on silica gel (eluent: hexane:ethyl acetate =3:1) to give methyl 7-methoxy-3-oxo-4-[3-(4-phenylpiperazin-1-yl)propyl]-3,4-dihydro-2H-1,5-benzoxathiepin-4-carboxylate. Recrystallization from methanol gives white crystals. m.p. of 110°-112° C. Yield of 2.1 g.

Provenance & Evidence