HRID2236185

反应详情

EQUATION

反应方程式

HRID 2236185 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-acetyl-4-cyclohexyl-but-2-enoic acid ethyl ester (1.79 g, 7.52 mmol) in 40 mL CCl4 was added to a slurry of NBS (1.338 g, 7.52 mmol) in 40 mL CCl4. The mixture was refluxed under argon for 12 hours, stirred at room temperature for 68 hours and then cooled in an ice bath. The precipitated solid was filtered off and the filtrate was evaporated to an oil that was purified by short-path distillation (165-185° C., 1 mm Hg) yielding 5-cyclohexyl-2-methyl-furan-3-carboxylic acid ethyl ester (1.36 g, 77%).

WORKUP

后处理

  1. temperatureThe mixture was refluxed under argon for 12 hours
  2. temperaturecooled in an ice bath
  3. filtrationThe precipitated solid was filtered off
  4. customthe filtrate was evaporated to an oil that
  5. distillationwas purified by short-path distillation (165-185° C., 1 mm Hg)