HRID11858
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
CONDITIONS
反应条件
- 温度
- 70 °C
PROCEDURE
实验过程
The compound obtained in Example 17-1 (269.9 mg) was dissolved in carbontetrachloride (8 ml), and N-bromosuccinimide (252.6 mg) and azobisisobutylonitrile (22.1 mg) were added to the solution. The mixture was stirred for 6 hours at 70° C. After the completion of the reaction, the solid was removed using a glass filter and the filtrate was concentrated. The residue was dissolved in chloroform and washed with 1 mol/l aqueous solution of sodium hydroxide and saturated brine. The solution was dried over anhydrous sodium sulfate. The solvent was removed by distillation and the residue was dried under reduced pressure to obtain the title compound (363.3 mg) as pale yellow oil.
WORKUP
后处理
- customAfter the completion of the reaction
- customthe solid was removed
- filtrationfilter
- concentrationthe filtrate was concentrated
- dissolutionThe residue was dissolved in chloroform
- washwashed with 1 mol/l aqueous solution of sodium hydroxide and saturated brine
- dry with materialThe solution was dried over anhydrous sodium sulfate
- customThe solvent was removed by distillation
- customthe residue was dried under reduced pressure