HRID1418616

反应详情

EQUATION

反应方程式

HRID 1418616 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of the compound (2.8 g) obtained in Example (54b) in methanol (15 ml) and 1N-HCl (6 ml) was heated for 2 hours under reflux. After removal of the solvent, the residue was made alkaline with an aqueous solution of NaHCO3, and the mixture was extracted with ethyl acetate. The extract was washed with water, dried over MgSO4 and concentrated to dryness. The residue was purified by column chromatography on silica gel, and the product was recrystallized from ethyl acetate-hexane to afford yellow needles (1.6 g, 73%).

WORKUP

后处理

  1. temperaturewas heated for 2 hours
  2. temperatureunder reflux
  3. customAfter removal of the solvent
  4. extractionthe mixture was extracted with ethyl acetate
  5. washThe extract was washed with water
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated to dryness
  8. customThe residue was purified by column chromatography on silica gel
  9. customthe product was recrystallized from ethyl acetate-hexane