HRID2216939

反应详情

EQUATION

反应方程式

HRID 2216939 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. temperatureis refluxed for 15 hours
  2. washThe reaction is monitored by means of thin layer chromatography (Polygram Sil G/UV254 prefabricated foils; eluting agent: petroleum ether:ethyl acetate (3:7))
  3. waitThe reaction mixture is stored over night in the refrigerator at approximately 5° C
  4. filtrationThe precipitate is filtered
  5. customrecrystallized from a mixture of ethanol and water