HRID2420257

反应详情

EQUATION

反应方程式

HRID 2420257 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Twenty grams of 1-benzoyl-4,5-epoxy-1,2,2a,3,4,5-hexahydrobenz[cd]indole were dissolved in 500 ml. of benzene. 7.7 g. of zinc iodide were added and the resulting mixture refluxed under nitrogen for about 1.5 hours. Thin layer chromatrography indicated one major spot slightly slower than the spot corresponding to starting material. The reaction mixture was cooled and then diluted with ethyl acetate. The resulting organic layer was washed with water, and with saturated aqueous sodium chloride and was then dried. Evaporation of the solvent yielded a residue comprising 1-benzoyl-4-keto-1,2,2a,3,4,5-hexahydrobenz[cd]indole formed in the above reaction. The residue was crystallized by trituration with ether containing a small amount of benzene, yielding crystals melting at 146°-149° C. (yield equals 16.9 g.)

WORKUP

后处理

  1. temperaturethe resulting mixture refluxed under nitrogen for about 1.5 hours
  2. temperatureThe reaction mixture was cooled
  3. washThe resulting organic layer was washed with water
  4. dry with materialwith saturated aqueous sodium chloride and was then dried
  5. customEvaporation of the solvent