反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
The compound (153 mg, 0.201 mmol) obtained in Example 89d was dissolved in 2 N hydrochloric acid-methanol (2.01 mL, 4.01 mmol), and the mixture was stirred at room temperature for 2 hours. Toluene was added to the reaction mixture, the solvent was evaporated under reduced pressure, the resulting residue was dissolved in ethyl acetate, and the mixture was adjusted to pH 10 with a 1 N aqueous sodium hydroxide solution. The mixture was extracted with ethyl acetate (×2) 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=100:0→methylene chloride:methanol=10:1, v/v) to give the title compound (122 mg; yield, 92%) as a white solid.
WORKUP
后处理
- customthe solvent was evaporated under reduced pressure
- dissolutionthe resulting residue was dissolved in ethyl acetate
- extractionThe mixture was extracted with ethyl acetate (×2)
- dry with materialdried with anhydrous sodium sulfate
- customThe solvent was evaporated under reduced pressure
- customthe resulting residue was purified by NH silica gel column chromatography (ethyl acetate