HRID347807
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
CONDITIONS
反应条件
- 温度
- 65 °C
PROCEDURE
实验过程
To a solution of ethyl (1S, 3R, 4R)-2-[(S)-1-phenylethyl]-2-azabicyclo[2.2.1]heptane-3-carboxylate (601 mg, 2.20 mmol) in tetrahydrofuran (12 ml)-methanol (6 ml) was added 1N sodium hydroxide (12 ml) and the mixture was stirred at 65° C. for 21 hours. The reaction mixture was neutralized and the water phase was concentrated. The residue was dissolved in chloroform and dried over magnesium sulfate. The solvent was evaporated and the residue was purified by silica gel column chromatography (0–15% methanol/chloroform), to give (1S, 3R, 4R)-2-[(S)-1-phenylethyl]-2-azabicyclo[2.2.1]heptane-3-carboxylic acid (445 mg, 83%).
WORKUP
后处理
- concentrationthe water phase was concentrated
- dissolutionThe residue was dissolved in chloroform
- dry with materialdried over magnesium sulfate
- customThe solvent was evaporated
- customthe residue was purified by silica gel column chromatography (0–15% methanol/chloroform)