HRID908604
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
4N Hydrogen chloride/1,4-dioxane solution (40 ml) was added to the compound (2.20 g) obtained in Step 3, and the mixture was stirred at room temperature for 1.5 hr. The reaction mixture was concentrated under reduced pressure, and the residue was partitioned by adding chloroform and saturated aqueous sodium hydrogen carbonate solution. The organic layer was dried over anhydrous sodium carbonate, filtrated, and concentrated under reduced pressure. The residue was crystallized from a mixed solvent of diisopropyl ether and n-hexane, collected by filtration and dried to give the title compound (1.57 g).
WORKUP
后处理
- concentrationThe reaction mixture was concentrated under reduced pressure
- customthe residue was partitioned
- additionby adding chloroform and saturated aqueous sodium hydrogen carbonate solution
- dry with materialThe organic layer was dried over anhydrous sodium carbonate
- filtrationfiltrated
- concentrationconcentrated under reduced pressure
- customThe residue was crystallized from a mixed solvent of diisopropyl ether and n-hexane
- filtrationcollected by filtration
- customdried