HRID426916

反应详情

EQUATION

反应方程式

HRID 426916 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 5'-hydroxy-spiro(cyclopentane-1,1'-indan)-3'-one (20.2 g; 0.1 mole), acetone (1000 ml), anhydrous potassium carbonate (37.5 g) and methyl iodide (50 ml) is refluxed for 5-6 hours. The mixture is evaporated to dryness, after which the residue is taken up in water and trichloroethylene. The trichloroetylene solution is extracted with 2×150 ml of 2 N sodium hydroxide and dried with anhydrous magnesium sulphate. The solvent is distilled off and a yellow oil is obtained, which soon crystallizes, yield 16 g (74%). After recrystallization from n-hexane the substance melts at 80° C.

WORKUP

后处理

  1. temperatureis refluxed for 5-6 hours
  2. customThe mixture is evaporated to dryness
  3. extractionThe trichloroetylene solution is extracted with 2×150 ml of 2 N sodium hydroxide
  4. dry with materialdried with anhydrous magnesium sulphate
  5. distillationThe solvent is distilled off
  6. customa yellow oil is obtained
  7. customwhich soon crystallizes
  8. customAfter recrystallization from n-hexane the substance melts at 80° C.