反应详情

A mixture of 3-acetylisoquinoline (1.01 g, 5.9 mmol) and 1-methyl-2-hydrazinobenzimidazole (0.96 g, 5.55 mmol) in 15 ml of methanol is stirred for approximately 7 days at room temperature after the addition of 5 drops of glacial acetic acid. The reaction is monitored by means of thin layer chromatography (Polygram Sil G/UV254 prefabricated foils; eluting agent: petroleum ether:ethyl acetate (3:7)). The reaction mixture is stored over night in the freezer at approximately −20° C. The precipitate is filtered, washed with ether and dried. The product is recrystallized from a mixture of ethylacetate and petroleum ether. Yield: 1.66 g (95% of theory).

1. washThe reaction is monitored by means of thin layer chromatography (Polygram Sil G/UV254 prefabricated foils; eluting agent: petroleum ether:ethyl acetate (3:7))
2. waitThe reaction mixture is stored over night in the freezer at approximately −20° C
3. filtrationThe precipitate is filtered
4. washwashed with ether
5. customdried
6. customThe product is recrystallized from a mixture of ethylacetate and petroleum ether