反应 #65205

ord-c3b85288842e4748a11fb74cde879943

反应条件

温度
130°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The organic layer was separated
  2. 2
    洗涤washed with water, 2N NaOH and water in the order
  3. 3
    workup.DISTILLATIONthe solvent was distilled off
  4. 4
    其他The residue was chromatographed on silica gel
  5. 5
    洗涤eluted with hexane-acetone (4:1)

实验过程

A mixture of 5-(2-chlorobenzoylamino)indan (16 g), 2-chlorobenzoyl chloride (15.5 g) and tin tetrachloride (10.2 ml) was heated at 130° C. for 30 minutes and, then, diluted with ethyl acetate (150 ml), followed by addition of 3N HCl (150 ml). The organic layer was separated and washed with water, 2N NaOH and water in the order mentioned and the solvent was distilled off. The residue was chromatographed on silica gel and eluted with hexane-acetone (4:1) to give 6-(2-chlorobenzoyl)-5-(2-chlorobenzoylamino)indan as oil (16.0 g, 66.2%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05418239uspto-grants-1995_05