HRID27301

反应详情

EQUATION

反应方程式

HRID 27301 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 4.2 g of trans-1-chloro-3-(3-ethyl-1-methylcyclobutyl)-prop-1-en-3-one (prepared in Example 5A) and 10 g of anhydrous sodium iodide in 60 ml of acetone was refluxed with about 0.5 ml H2SO4 for 4 hr under an argon atmosphere. The solvent was removed by evaporation in vacuo. The residue was diluted with water and the aqueous mixture was extracted several times with ether. The combined ether extract was washed with aqueous sodium thiosulfate solution and then dried over anhydrous magnesium sulfate and evaporated in vacuo to yield 6.8 g of the title compound having the following physical characteristics:

WORKUP

后处理

  1. customThe solvent was removed by evaporation in vacuo
  2. additionThe residue was diluted with water
  3. extractionthe aqueous mixture was extracted several times with ether
  4. extractionThe combined ether extract
  5. washwas washed with aqueous sodium thiosulfate solution
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customevaporated in vacuo