反应详情

温度

102.5 °C

A mixture of 6-(5-amino-6-bromo-3-phenyl-2-pyrazinyl)-2-isopropyl-3(2H)-pyridazinone (11.35 g) and sodium thiomethoxide (4.12 g) in 1,3-dimethyl-2-imidazolidinone (17 ml) was heated at 100-105° C. for one hour. The mixture was poured into water (170 ml). The precipitate was collected by filtration, dissolved in CHCl3, dried over MgSO4, concentrated under reduced pressure to give a residue. The residue was purified by column chromatography on silica gel eluting with a mixture of n-hexane and EtOAc (50:50 v/v) to give 6-[5-amino-6-(methylthio)-3-phenyl-2-pyrazinyl]-2-isopropyl-3(2H)-pyridazinone as a solid (4.32 g).

1. filtrationThe precipitate was collected by filtration
2. dissolutiondissolved in CHCl3
3. dry with materialdried over MgSO4
4. concentrationconcentrated under reduced pressure
5. customto give a residue
6. customThe residue was purified by column chromatography on silica gel eluting with a mixture of n-hexane and EtOAc (50:50 v/v)