HRID1589731

反应详情

EQUATION

反应方程式

HRID 1589731 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2,5 Dimethylthiophene (50 g, 0.446 mole) and cyclopropylcarbonyl chloride (54.36 g, 0.52 mole) were dissolved in dichloromethane (500 ml) and cooled in an ice bath. Tin(IV) chloride (122.44 g, 0.470 mole) in dichloromethane (150 ml) was added slowly over 1 hour with stirring to form a deep red solution. The mixture was warmed to room temperature and stirred for a further hour. The mixture was then poured into cold water (750 ml) and stirred rapidly for 30 min. The dichloromethane layer was washed with cold water and dried over magnesium sulfate. The dichloromethane solvent was removed to give the ketone, 2,5-dimethyl-3-thienyl cyclopropyl ketone, as a brown oil (73.25 g).

WORKUP

后处理

  1. temperaturecooled in an ice bath
  2. customto form a deep red solution
  3. stirringstirred for a further hour
  4. stirringstirred rapidly for 30 min
  5. washThe dichloromethane layer was washed with cold water
  6. dry with materialdried over magnesium sulfate
  7. customThe dichloromethane solvent was removed