HRID971863

反应详情

EQUATION

反应方程式

HRID 971863 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Twenty grams of ethyl 2-[4-(1-ethoxycarbonyl-2-oxocyclopentan-1-ylmethyl)phenyl]propionate was dissolved in 30 ml of dioxane and 100 ml of 47% hydrobromic acid and the solution was refluxed for 6 hours. The reaction mixture was then extracted with ether, the extract was washed with water, dried over anhydrous sodium sulfate, and the solvent removed by distillation to give an yellow oily substance. The product was subjected to a vacuum distillation to yield 13.1 g of the desired compound as a colorless oily substance, b.p. 190°-195° C. at 0.3 mm Hg (bath temp.). The compound solidified as it was cooled to crystals, m.p. 108.5°-111° C.

WORKUP

后处理

  1. extractionThe reaction mixture was then extracted with ether
  2. washthe extract was washed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. customthe solvent removed by distillation
  5. customto give an yellow oily substance
  6. distillationThe product was subjected to a vacuum distillation