HRID2414319

反应详情

EQUATION

反应方程式

HRID 2414319 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Iron powder (1.5 g) was added to a solution of the product from step (i) (1.37 g) in acetic acid (50 ml) and tetrahydrofuran (20 ml). After stirring at room temperature for 5 h, the mixture was filtered through celite, the solvent removed under reduced pressure and the residue partitioned between ethyl acetate and aqueous sodium hydrogencarbonate solution. The organic layer was washed with water, dried and evaporated under reduced pressure. Purification was by chromatography eluting with 50% ethyl acetate/isohexane. Yield 1.05 g.

WORKUP

后处理

  1. filtrationthe mixture was filtered through celite
  2. customthe solvent removed under reduced pressure
  3. customthe residue partitioned between ethyl acetate and aqueous sodium hydrogencarbonate solution
  4. washThe organic layer was washed with water
  5. customdried
  6. customevaporated under reduced pressure
  7. customPurification
  8. washeluting with 50% ethyl acetate/isohexane