反应详情

4-Chloro-2-methylpyridine hydrochloride (941 mg), triethylamine (1.93 g) and ethanol (50 ml) were added to 4-benzyloxycarbonyl-1-[(4-ethoxycarbonylamino-4-piperidinyl)methyl]-2-piperazinone (2.0 g), and the mixture was reacted at 150° C. for 10 hours in a sealed tube. The reaction mixture was concentrated, a 10% aqueous sodium carbonate solution was added to the residue, and the mixture was extracted with dichloromethane, dried, and concentrated. The resulting residue was purified by column chromatography (dichloromethane:10% aqueous ammonia-containing methanol=20:1) to obtain the colorless amorphous title compound (1.31 g).

1. customthe mixture was reacted at 150° C. for 10 hours in a sealed tube
2. concentrationThe reaction mixture was concentrated
3. additiona 10% aqueous sodium carbonate solution was added to the residue
4. extractionthe mixture was extracted with dichloromethane
5. customdried
6. concentrationconcentrated
7. customThe resulting residue was purified by column chromatography (dichloromethane:10% aqueous ammonia-containing methanol=20:1)