HRID383142

反应详情

EQUATION

反应方程式

HRID 383142 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of DL, 2-hydroxy-4-methylmercaptobutyric acid calcium salt (2.2 g) in 0.5M HCl (50 mL) was saturated with sodium chloride, extracted exhaustively with EtOAc, which was dried (MgSO4), filtered and concentrated. The residue was dissolved in methanol (10 mL) and trimethylsilyldiazomethane (2M in hexane) was added until the yellow color persisted for 30 min. The reaction was quenched by addition of glacial acetic acid and concentrated. The residue was purified by silica gel chromatography eluting with 30% EtOAc/hexane to give the title compound as a light yellow oil (1.37 g).

WORKUP

后处理

  1. extractionextracted exhaustively with EtOAc, which
  2. dry with materialwas dried (MgSO4)
  3. filtrationfiltered
  4. concentrationconcentrated
  5. dissolutionThe residue was dissolved in methanol (10 mL)
  6. additiontrimethylsilyldiazomethane (2M in hexane) was added until the yellow color
  7. customThe reaction was quenched by addition of glacial acetic acid
  8. concentrationconcentrated
  9. customThe residue was purified by silica gel chromatography
  10. washeluting with 30% EtOAc/hexane