HRID1444559

反应详情

EQUATION

反应方程式

HRID 1444559 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturecooled on ice
  2. customThe reaction mixture was removed
  3. temperaturefrom cooling
  4. customThe solvent was then removed by rotary evaporation
  5. additionThe residue was treated with water (100 mL)
  6. extractionThe product was extracted with ethyl acetate (300 mL, 200 mL)
  7. customEvaporation of the solvent and crystallization of the residue from methylene chloride/hexane