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
2(S)-Benzyloxycarbonylamino-3-(2,6-difluorophenyl)propionic acid methyl ester (5 g, 14.4 mmol) was dissolved in methanol (60 mL) and cooled on ice. 1 N NaOH (22 mL, 22 mmol) was added dropwise over 15 min. The reaction mixture was removed from cooling and continue stirring at room temperature for 4 h. The solvent was then removed by rotary evaporation. The residue was treated with water (100 mL) and then with 1 N HCl to adjust the pH to 4. The product was extracted with ethyl acetate (300 mL, 200 mL). Evaporation of the solvent and crystallization of the residue from methylene chloride/hexane gave 2(S)-benzyloxycarbonylamino-3-(2,6-difluoro-phenyl)propionic acid (4.6 g, 13.7 mmol, 94% yield).
WORKUP
后处理
- temperaturecooled on ice
- customThe reaction mixture was removed
- temperaturefrom cooling
- customThe solvent was then removed by rotary evaporation
- additionThe residue was treated with water (100 mL)
- extractionThe product was extracted with ethyl acetate (300 mL, 200 mL)
- customEvaporation of the solvent and crystallization of the residue from methylene chloride/hexane