HRID617165

反应详情

EQUATION

反应方程式

HRID 617165 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 20 ml of ethanol was dissolved 2.10 g (3.32 mmol) of Compound 54 obtained in Example 54, excess sodium borohydride was added, and the mixture was stirred under heating at reflux for 1 hour. After cooling, the solvent was removed, water was added and the mixture was subjected to extraction with ethyl acetate. The organic layer was washed with sodium chloride solution, dried and concentrated to give residue. The residue was purified by silica gel column chromatography(eluent: chloroform/methanol=100/1) and recrystallized from ethanol to give 1.29 g (yield: 66%) of Compound 55 as white crystals.

WORKUP

后处理

  1. additionwas added
  2. temperatureunder heating
  3. temperatureat reflux for 1 hour
  4. temperatureAfter cooling
  5. customthe solvent was removed
  6. additionwater was added
  7. extractionthe mixture was subjected to extraction with ethyl acetate
  8. washThe organic layer was washed with sodium chloride solution
  9. customdried
  10. concentrationconcentrated
  11. customto give residue
  12. customThe residue was purified by silica gel column chromatography(eluent
  13. customchloroform/methanol=100/1) and recrystallized from ethanol