HRID2216939
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of cyclohexyl-(2-pyridyl)-methanone (0.77 g, 4.05 mmol) and 2-hydrazinobenzothiazole (0.60 g, 4.02 mmol) in 15 ml of methanol is refluxed for 15 hours 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 refrigerator at approximately 5° C. The precipitate is filtered and recrystallized from a mixture of ethanol and water. Yield: 1.09 g (80% of theory).
WORKUP
后处理
- temperatureis refluxed for 15 hours
- washThe reaction is monitored by means of thin layer chromatography (Polygram Sil G/UV254 prefabricated foils; eluting agent: petroleum ether:ethyl acetate (3:7))
- waitThe reaction mixture is stored over night in the refrigerator at approximately 5° C
- filtrationThe precipitate is filtered
- customrecrystallized from a mixture of ethanol and water