反应详情

(Method C) 4-(6-Chloronaphthalene-2-sulfonyl)-1-[1-(4-pyridyl)-4-piperidinylamino]-2-piperazinone (90 mg) was dissolved in a 37% aqueous solution of formaldehyde (2.9 ml) and formic acid (1.4 ml) and refluxed for 15 hours. The reaction mixture was cooled, made alkaline by adding 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) to obtain the title compound (38 mg) as colorless crystals.

1. temperaturerefluxed for 15 hours
2. temperatureThe reaction mixture was cooled
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)