HRID446534

反应详情

EQUATION

反应方程式

HRID 446534 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Lithium borohydride (39 mg, 1.80 mmol) was suspended in tetrahydrofuran (6 mL), methanol (73 μL, 1.80 mmol) and a solution of the compound (235 mg, 0.450 mmol) obtained in Example 39a in tetrahydrofuran (7 mL) was added, and the mixture was stirred at room temperature for 2 days. A 1 N aqueous sodium hydroxide solution was added to the reaction mixture, and the mixture was extracted with ethyl acetate (×3). The organic layer was washed with saturated sodium chloride solution and dried with anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the resulting residue was purified by NH silica gel column chromatography (ethyl acetate:methanol=50:1, v/v) to give the title compound (163 mg; yield, 75%) as a white solid.

WORKUP

后处理

  1. extractionthe mixture was extracted with ethyl acetate (×3)
  2. washThe organic layer was washed with saturated sodium chloride solution
  3. dry with materialdried with anhydrous sodium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. customthe resulting residue was purified by NH silica gel column chromatography (ethyl acetate:methanol=50:1, v/v)