HRID279146
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe mixture was refluxed for 1 hour
- temperatureThe mixture was cooled in an ice bath
- customwas removed with an evaporator
- dissolutionThe residue was dissolved in ethyl acetate (60 ml)
- extractionextracted with 5% NaHCO3 solution (2×30 ml) and water (30 ml)
- dry with materialThe organic phase was dried over Na2SO4
- customevaporated