反应详情

1-{[1-(tert-Butoxycarbonyl)piperidinyl]methylamino}-4-(6-chloronaphthalene-2-sulfonyl)-2-piperazinone (1.63 g) was combined with methanol (10 ml) and a 4N solution of hydrochloric acid in ethyl acetate (15 ml) and stirred at room temperature for 30 minutes. The reaction mixture was concentrated and the residue obtained was combined with 4-chloropyridine hydrochloride (950 mg), triethylamine (3.8 g) and ethanol (100 ml), and reacted in a sealed tube at 150° C. for 15 hours. The reaction mixture was concentrated and the residue was combined with a 1N aqueous solution of sodium hydroxide, extracted with dichloromethane, dried and concentrated. The residue obtained was purified by a column chromatography (dichloromethane: 10% aqueous ammonia-containing methanol=20:1) and crystallized from ether to obtain the title compound (794 mg) as colorless crystals.

1. concentrationThe reaction mixture was concentrated
2. customthe residue obtained
3. customreacted in a sealed tube at 150° C. for 15 hours
4. concentrationThe reaction mixture was concentrated
5. extractionextracted with dichloromethane
6. customdried
7. concentrationconcentrated
8. customThe residue obtained
9. customwas purified by a column chromatography (dichloromethane: 10% aqueous ammonia-containing methanol=20:1)
10. customcrystallized from ether