HRID908604

反应详情

EQUATION

反应方程式

HRID 908604 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customthe residue was partitioned
  3. additionby adding chloroform and saturated aqueous sodium hydrogen carbonate solution
  4. dry with materialThe organic layer was dried over anhydrous sodium carbonate
  5. filtrationfiltrated
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was crystallized from a mixed solvent of diisopropyl ether and n-hexane
  8. filtrationcollected by filtration
  9. customdried