反应详情

温度

50 °C

4.12 Grams of 2-(4-chlorobenzoyl)ethyl chloride and 6.08 g of sodium iodide were dispersed in 50 ml of dimethylformamide, and heated at 50° C. for 1.5 hours. Then, to this dispersion was added 50 ml of dimethylformamide solution containing 3 g of 6-(1-piperazinylcarbonyl)-3,4-dihydrocarbostyril, and further 9.8 g of potassium carbonate was added thereto and reacted by heating at 70° C. for 3 to 4 hours. After the reaction was completed, the insoluble matters were removed by filtration, and the solvent in the filtrate was removed by evaporation under reduced pressure. The residue thus obtained was extracted with chloroform, and the extract was dried with anhydrous calcium sulfate, then concentrated. The thus obtained residue was purified by means of a silica gel column chromatography (eluent: dichloromethane:methanol=50:1), then recrystallized from ethanol-diethyl ether to yield 2.29 g of 6-{4-[2-(4-chlorobenzoyl)ethyl]-1-piperazinylcarbonyl}-3,4-dihydrocarbostyril. White powdery substance.

1. additionwas added
2. customreacted
3. temperatureby heating at 70° C. for 3 to 4 hours
4. customthe insoluble matters were removed by filtration
5. customthe solvent in the filtrate was removed by evaporation under reduced pressure
6. customThe residue thus obtained
7. extractionwas extracted with chloroform
8. dry with materialthe extract was dried with anhydrous calcium sulfate
9. concentrationconcentrated
10. customThe thus obtained residue was purified by means of a silica gel column chromatography (eluent: dichloromethane:methanol=50:1)
11. customrecrystallized from ethanol-diethyl ether