HRID413677

反应详情

EQUATION

反应方程式

HRID 413677 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The above ester (3.5 g, 8.7 mmol) was dissolved in ethanol (40 ml). 5 N Sodium hydroxide (4 ml) was added and the mixture was allowed to stand for 3 days. Ethanol was evaporated in vacuo and the residue was dissolved in water (50 ml). The solution was washed with diethyl ether (30 ml) and acetic acid (3 ml) was added to the aqueous phase which subsequently was extracted with dichloromethane (50 ml). The organic phase was dried (MgSO4) and the solvent was evaporated in vacuo. The residue was filtered through silica gel (20 g) using ethanol as eluent. The solvent was evaporated and acetone was added to the residue. The solid was isolated by filtration and dried to give 1.8 g (55%) of the title compound.

WORKUP

后处理

  1. customEthanol was evaporated in vacuo
  2. dissolutionthe residue was dissolved in water (50 ml)
  3. washThe solution was washed with diethyl ether (30 ml) and acetic acid (3 ml)
  4. additionwas added to the aqueous phase which
  5. extractionsubsequently was extracted with dichloromethane (50 ml)
  6. dry with materialThe organic phase was dried (MgSO4)
  7. customthe solvent was evaporated in vacuo
  8. filtrationThe residue was filtered through silica gel (20 g)
  9. customThe solvent was evaporated
  10. additionacetone was added to the residue
  11. customThe solid was isolated by filtration
  12. customdried