HRID1525574

反应详情

EQUATION

反应方程式

HRID 1525574 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

Under protective gas (Ar), 10 ml of 2 molar aqueous sodium hydroxide solution were added to 1.75 g (5.55 mmol) of methyl 4-cyano-3-(4-fluorophenyl)-4-(3-fluorophenyl)butanoate (Example A1) in 50.0 ml of methanol, and the mixture was stirred at 25° C. for 8 h. The methanol was removed under reduced pressure. The residue was acidified with concentrated hydrochloric acid (pH=3) and extracted three times with in each case 15 ml of dichloromethane. The combined organic phases were dried over sodium sulphate and the solvent was removed under reduced pressure. This gave 1.62 g (96.9% of theory) of the title compound in the form of colourless crystals (erythro:threo=49:51 according to comparison of the multiplets in the 1H-NMR in CDCl3 at 2.60 and 2.85 ppm).

WORKUP

后处理

  1. customThe methanol was removed under reduced pressure
  2. extractionextracted three times with in each case 15 ml of dichloromethane
  3. dry with materialThe combined organic phases were dried over sodium sulphate
  4. customthe solvent was removed under reduced pressure