HRID703279

反应详情

EQUATION

反应方程式

HRID 703279 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
45 °C

PROCEDURE

实验过程

In a 100 ml-volume autoclave whose atmosphere had been displaced with nitrogen was added a methylene chloride solution of 2.5 g of methyl 2-(N-benzoylamino)methyl-3-oxobutanoate and 84.5 mg (0.05 mmole) of Ru2Cl4 ((-)-BINAP2 (NEt3), and a reaction was conducted by stirring at 45° C. under a hydrogen pressure of 70 kg/cm2 for 24 hours. The reaction mixture was taken out, and the solvent was removed by distillation under reduced pressure of 20 mmHg at 30° C. The residue was purified by silica gel column chromatography using a 7/3 (by volume) mixture of hexane and isopropanol as an eluent to obtain 2.27 g (yield: 91%) of methyl (2R, 3S)-2-(N-benzoylamino)methyl-3-hydroxybutanoate having an optical purity of 97 %ee.

WORKUP

后处理

  1. customthe solvent was removed by distillation under reduced pressure of 20 mmHg at 30° C
  2. customThe residue was purified by silica gel column chromatography
  3. additiona 7/3 (by volume) mixture of hexane and isopropanol as an eluent