反应详情

To sodium bicarbonate solution were added 4-(5-chlorobenzofuran-2-sulfonyl)-1-(piperidin-4-ylmethyl)-2-piperazinone hydrochloride (215 mg) and chloropyridine hydrochloride (144 mg), and the mixture was extracted with dichloromethane (twice), dried and concentrated. To the residue was added isoamylalcohol (15 ml), and the mixture was allowed to react at 130° C. for 15 hours. The reaction solution was concentrated, and the residue was dissolved in dichloromethane. The solution was washed with 1N sodium hydroxide solution, dried and concentrated, and the residue was purified with silica gel column chromatography (dichloromethane:methanol containing 10% ammonia solution 15:1) to give colorless solid of 4-(5-chlorobenzofuran-2-sulfonyl)-1-[1-(4-pyridyl)piperidin-4-ylmethyl]-2-piperazinone (87 mg), which was treated with hydrochloric acid to give colorless solid of the title compound (80 mg) as hydrochloride salt.

1. extractionthe mixture was extracted with dichloromethane (twice),
2. customdried
3. concentrationconcentrated
4. additionTo the residue was added isoamylalcohol (15 ml)
5. customto react at 130° C. for 15 hours
6. concentrationThe reaction solution was concentrated
7. dissolutionthe residue was dissolved in dichloromethane
8. washThe solution was washed with 1N sodium hydroxide solution
9. customdried
10. concentrationconcentrated
11. customthe residue was purified with silica gel column chromatography (dichloromethane:methanol containing 10% ammonia solution 15:1)