HRID21445

反应详情

EQUATION

反应方程式

HRID 21445 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1-[2-chloro-4-(methylsulphenyl)phenyl]-3-cyclopropylprop-1-yn-3-one (1.39g) and ethyl chloro-oximidoacetate (0.84g) in toluene was stirred and heated at reflux overnight. It was cooled and evaporated to dryness. The residue was purified by chromatography eluted with a mixture of hexane and dichloromethane, followed by ether to give ethyl 5-[2-chloro-4-(methylsulphenyl)phenyl]-4-cyclopropylcarbonylisoxazole-3-carboxylate (compound 9, 0.72g) as an orange solid, m.p. 50° C.

WORKUP

后处理

  1. temperatureheated
  2. temperatureat reflux overnight
  3. temperatureIt was cooled
  4. customevaporated to dryness
  5. customThe residue was purified by chromatography
  6. washeluted with a mixture of hexane and dichloromethane