HRID1424093

反应详情

EQUATION

反应方程式

HRID 1424093 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of the compound (33.1 g, 62.0 mmol) obtained in Example 60-4) in tetrahydrofuran (500 mL), tetrabutylammonium fluoride (74.4 mL, 1 M tetrahydrofuran solution) was added, and the mixture was stirred at room temperature for 1.5 h. Saturated aqueous sodium hydrogencarbonate was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated sodium chloride solution and then dried with anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. The concentrated residue was purified by silica gel column chromatography (ethyl acetate:methanol=4:1) to obtain the title compound (22.5 g, 87%) as a white solid.

WORKUP

后处理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with saturated sodium chloride solution
  3. dry with materialdried with anhydrous sodium sulfate
  4. distillationthe solvent was distilled off under reduced pressure
  5. customThe concentrated residue was purified by silica gel column chromatography (ethyl acetate:methanol=4:1)