HRID259293

反应详情

EQUATION

反应方程式

HRID 259293 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of acryloyl ferrocene (2.16g) and cyclohexylmercaptan (1.16g) in ethanol (50 ml) was set aside at ambient temperature for 24 hours. Evaporation of the ethanol gave an oil which was dissolved in chloroform (100 ml). The chloroform solution was washed successively with aqueous sodium hydroxide and water, dried over sodium sulphate and evaporated affording crude product. This was chromatographed through a silica-gel column (66g) using initially 1% ethyl acetate/petroleum ether (60°-80°) then 3% ethyl acetate/petroleum ether as eluent. This afforded an oil which crystallised on cooling and trituration with petroleum ether. The solid was filtered off, washed well with petroleum ether and dried giving the title compound, m.p. 46.5°-48.5°to C.

WORKUP

后处理

  1. customEvaporation of the ethanol
  2. customgave an oil which
  3. washThe chloroform solution was washed successively with aqueous sodium hydroxide and water
  4. dry with materialdried over sodium sulphate
  5. customevaporated
  6. customaffording crude product
  7. customThis was chromatographed through a silica-gel column (66g)
  8. custom1% ethyl acetate/petroleum ether (60°-80°)
  9. customThis afforded an oil which
  10. customcrystallised
  11. temperatureon cooling
  12. filtrationThe solid was filtered off
  13. washwashed well with petroleum ether
  14. customdried