反应详情

A mixture of 7-(3-chloropropoxy)-4H-benzopyran-4-one as prepared above in Preparation I (2.38 g; 10 mmol), 1-(2-chlorophenyl)piperazine dihydrochloride (2.96 g; 11 mmol), sodium bicarbonate (3 g; 35 mmol), sodium iodide (0.1 g; 0.6 mmole) in 50 ml dimethylformamide was mechanically stirred and heated at 85°-90° C. for seven hours. The solvent was then evaporated in vacuo and the residue partitioned between water and dichloromethane. The organic phase was treated with an excess of 10% HCl solution in methanol, evaporated in vacuo and the residue recrystallized from ethanol/ethyl acetate to yield 3.2 g of 7-[3-(4-(2-chlorophenyl)-1-piperazinyl)propoxy]-4H-1-benzopyran-4-one as its hydrochloride salt, mp 201°-203° C. (dec).

1. temperatureheated at 85°-90° C. for seven hours
2. customThe solvent was then evaporated in vacuo
3. customthe residue partitioned between water and dichloromethane
4. additionThe organic phase was treated with an excess of 10% HCl solution in methanol
5. customevaporated in vacuo
6. customthe residue recrystallized from ethanol/ethyl acetate