反应详情

A suspension of 3-[bis(4-methoxybenzyl)amino]-6-(1-isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-5-phenyl-2-pyrazinecarbonitrile (3.00 g) in a mixture of 2N aq. NaOH (30 ml) and dioxane (21 ml) was refluxed for 36 hours. After cooling, the mixture was extracted with EtOAc, dried over MgSO4, concentrated under reduced pressure and purified by column chromatography on silica gel eluting with a mixture of n-hexane and EtOAc (20:80 v/v) to give a solid. The solid was crystallized from a mixture of n-hexane and acetone to give 3-[bis(4-methoxybenzyl)amino]-6-(1-isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-5-phenyl-2-pyrazinecarboxamide (2.56 g).

1. temperaturewas refluxed for 36 hours
2. temperatureAfter cooling
3. extractionthe mixture was extracted with EtOAc
4. dry with materialdried over MgSO4
5. concentrationconcentrated under reduced pressure
6. custompurified by column chromatography on silica gel eluting with a mixture of n-hexane and EtOAc (20:80 v/v)
7. customto give a solid
8. customThe solid was crystallized from a mixture of n-hexane and acetone