反应详情

(3S)-3-(tert-Butoxycarbonylamino)-1-[1-(4-pyridyl)-4-piperidinylideneamino]-2-pyrrolidone (3.57 g) was dissolved in methanol (40 ml), combined with acetic acid (2.05 g) with cooling on ice, followed by sodium cyanoborohydride (807 mg) and stirred at room temperature for 30 minutes. The reaction mixture was concentrated, and the residue was combined with an aqueous solution of sodium hydroxide, extracted with dichloromethane, dried, concentrated, and purified by a column chromatography (dichloromethane: 10% aqueous ammonia-containing methanol=20:1) to obtain the title compound (2.56 g) as a colorless amorphous material.

1. temperaturewith cooling on ice
2. concentrationThe reaction mixture was concentrated
3. extractionextracted with dichloromethane
4. customdried
5. concentrationconcentrated
6. custompurified by a column chromatography (dichloromethane: 10% aqueous ammonia-containing methanol=20:1)