HRID279146

反应详情

EQUATION

反应方程式

HRID 279146 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1,2,3,4,4a,9a-Hexahydrofluoren-9-one (9.6 g) was dissolved in acetic anhydride (40 ml). p-Toluenesulfonic acid (1 g) was added and the mixture was refluxed for 1 hour. The mixture was cooled in an ice bath and water (20 ml) was added. After stirring for 20 minutes solvent was removed with an evaporator. The residue was dissolved in ethyl acetate (60 ml) and extracted with 5% NaHCO3 solution (2×30 ml) and water (30 ml). The organic phase was dried over Na2SO4 and evaporated. Yield was 10.9 g.

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 1 hour
  2. temperatureThe mixture was cooled in an ice bath
  3. customwas removed with an evaporator
  4. dissolutionThe residue was dissolved in ethyl acetate (60 ml)
  5. extractionextracted with 5% NaHCO3 solution (2×30 ml) and water (30 ml)
  6. dry with materialThe organic phase was dried over Na2SO4
  7. customevaporated