反应详情

A mixture of 4-acetyl pyrimidine (0.412 g, 3.37 mmol) and 2-hydrazinobenzimidazole (0.50 g, 3.37 mmol) in 15 ml of methanol is refluxed after the addition of 5 drops of glacial acetic acid, until monitoring of the reaction by means of thin layer chromatography (Polygram Sil G/UV254 prefabricated foils; eluting agent: CH2Cl2:MeOH (10:1)) did not reveal any further reaction. The reaction mixture is stored over night in the refrigerator at approximately 5° C. The precipitate is filtered and recrystallized from a mixture of ethyl acetate and diisopropyl ether. Yield: 0.65 g (76% of theory).

1. temperatureis refluxed
2. customuntil monitoring of the reaction
3. washby means of thin layer chromatography (Polygram Sil G/UV254 prefabricated foils; eluting agent: CH2Cl2:MeOH (10:1))
4. customany further reaction
5. waitThe reaction mixture is stored over night in the refrigerator at approximately 5° C
6. filtrationThe precipitate is filtered
7. customrecrystallized from a mixture of ethyl acetate and diisopropyl ether