HRID446563

反应详情

EQUATION

反应方程式

HRID 446563 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The compound (595 mg, 0.901 mmol) obtained in Example 68b was dissolved in tetrahydrofuran (12 mL), a 1 N aqueous sodium hydroxide solution (1.03 mL, 1.03 mmol), water (0.3 mL) and methanol (4 drops) were added, and the mixture was stirred at room temperature. After the reaction was completed, 1 N hydrochloric acid and water were added, the mixture was extracted with methylene chloride, and the resulting organic layer was dried with anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the resulting residue was purified by reverse phase liquid chromatography (XTerra Prep MS C18 OBD, 5 μm, 30×100 mm) (acetonitrile:0.1% aqueous ammonium acetate solution, 10:90→100:0, v/v) to give the title compound (233 mg; yield, 40%).

WORKUP

后处理

  1. extractionthe mixture was extracted with methylene chloride
  2. dry with materialthe resulting organic layer was dried with anhydrous sodium sulfate
  3. customThe solvent was evaporated under reduced pressure
  4. customthe resulting residue was purified by reverse phase liquid chromatography (XTerra Prep MS C18 OBD, 5 μm, 30×100 mm) (acetonitrile