HRID1796150

反应详情

EQUATION

反应方程式

HRID 1796150 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of (S)-3-Acetoxy-4-morpholin-4-yl-4-oxo-butyric acid and 2-Acetoxy-4-morpholin-4-yl-4-oxo-butyric acid (11 g, 44.8 mmol) in dry methanol (30 mL) HCl in dioxane (4M, 7.3 ml, 29.16 mmol) was added and stirred at room temperature for 5 hrs. The reaction mixture was neutralized with solid NaHCO3, filtered through a mixture of Celite/Na2SO4 (1:1) and concentrated under reduced pressure. Column chromatography on silica eluting with a mixture of ethyl acetate and methylene chloride gave (S)-3-Hydroxy-4-morpholin-4-yl-4-oxo-butyric acid methyl ester (6 g).

WORKUP

后处理

  1. additionwas added
  2. filtrationfiltered through a mixture of Celite/Na2SO4 (1:1)
  3. concentrationconcentrated under reduced pressure
  4. additionColumn chromatography on silica eluting with a mixture of ethyl acetate and methylene chloride