反应详情

温度

102.5 °C

To a suspension of 3-amino-6-(1-isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-5-phenyl-2-pyrazinecarbonitrile (665 mg) and thioacetamide (451 mg) in DMF (3.2 ml) was added a 4N hydrogen chloride solution of dioxane (3.2 ml) and the mixture was stirred at 100-105° C. for 2 hours. Water (65 ml) was added to the mixture to yield a precipitate. The precipitate was collected by filtration, subjected to column chromatography on silica gel eluting with a mixture of n-hexane and EtOAc (40:60 v/v) to give a solid. The solid triturated with acetone and collected by filtration to give 3-amino-6-(1-isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-5-phenyl-2-pyrazinecarbothioamide as a solid (417 mg).

1. customto yield a precipitate
2. filtrationThe precipitate was collected by filtration
3. additionsubjected to column chromatography on silica gel eluting with a mixture of n-hexane and EtOAc (40:60 v/v)
4. customto give a solid
5. customThe solid triturated with acetone
6. filtrationcollected by filtration