HRID2235245

反应详情

EQUATION

反应方程式

HRID 2235245 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Add 5 N NaOH solution (3 mL, 3 mmol) into 4-[4-chloro-3-(1-cyclohexyl-2-oxo-pyrrolidin-3-ylmethyl)-2-fluoro-phenyl]-butyric acid ethyl ester (Preparation 79) (0.58 g, 1.4 mmol) in methanol (5 mL) at room temperature and stir for 30 minutes. Evaporate MeOH under reduced pressure and neutralize the residue by 1N HCl. Extract the mixture with ethyl acetate (10 mL) and separate the organic layer. Dry the organic layer with magnesium sulfate, filter and evaporate solvent under reduced pressure. Purify the residue by column chromatography to obtain the title product as white solid (300 mg, 55%): Mass spectrum (ion spray): m/z=396.0 (M+H).

WORKUP

后处理

  1. extractionExtract the mixture with ethyl acetate (10 mL)
  2. customseparate the organic layer
  3. dry with materialDry the organic layer with magnesium sulfate
  4. filtrationfilter
  5. customevaporate solvent under reduced pressure
  6. customPurify the residue by column chromatography