反应详情

温度

50 °C

A solution of 4-(6-chloronaphthalene-2-sulfonyl)-1-[1-(4-pyridyl)-4-piperidinylideneamino]-2-piperazinone (120 mg) in trifluoroacetic acid (1 ml) was combined with triethylsilane (60 mg) and stirred at 50° C. for 4 hours. The reaction mixture was concentrated and the residue was combined with an ice-cooled 1 N aqueous solution of sodium hydroxide, extracted with dichloromethane, dried and then concentrated. The residue obtained was purified by a column chromatography (dichloromethane: 10% aqueous ammonia-containing methanol=20:1) and crystallized from acetone to obtain the title compound (88 mg) as colorless crystals.

1. concentrationThe reaction mixture was concentrated
2. temperaturecooled 1 N aqueous solution of sodium hydroxide
3. extractionextracted with dichloromethane
4. customdried
5. concentrationconcentrated
6. customThe residue obtained
7. customwas purified by a column chromatography (dichloromethane: 10% aqueous ammonia-containing methanol=20:1)
8. customcrystallized from acetone