反应 #93539

ord-3b7073b3151c4a99bac17ba77a9f95d0

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    洗涤washed with water and saturated saline
  2. 2
    干燥dried over magnesium sulfate
  3. 3
    workup.DISTILLATIONthe solvent was then distilled off
  4. 4
    其他The crude product thus obtained
  5. 5
    其他was purified by a silica gel column chromatography

实验过程

To a solution of 600 mg of β-(p-chlorophenyl)-α-methylene-γ-butyrolactone in 10 ml of toluene were added 0.44 ml of thiobenzoic acid and one drop of triethylamine and the reaction was effected at room temperature for 18 hours. The reaction mixture was diluted with 100 ml of ethyl ether, washed with water and saturated saline, dried over magnesium sulfate and the solvent was then distilled off. The crude product thus obtained was purified by a silica gel column chromatography to give 750 mg (yield 75%) of the title compound.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04613613uspto-grants-1986_09