HRID703278

反应详情

EQUATION

反应方程式

HRID 703278 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a 100 ml-volume stainless steel autoclave whose atmosphere had been displaced with nitrogen was added a solution of 2.5 g (10 mmole) of methyl 2-(N-benzoylamino)methyl-3-oxobutanoate and 184 mg (0.1 mmole) of [Ru((+)BINAP)](CLO4)2 in 18 ml of dichloroethane, and a reaction was conducted at 70° C. under a hydrogen pressure of 100 kg/cm2 for 30 hours. The reaction mixture was concentrated under reduced pressure of 20 mmHg, and the residue was purified by silica gel column chromatography using a 7/3 (by volume) mixture of hexane and isopropanol as an eluent to give 2.19 g (yield: 86.5%) of methyl (2S, 3R)-2-(N-benzoylamino)methyl-3-hydroxybutanoate having an optical purity of 90 %ee.

WORKUP

后处理

  1. customwas conducted at 70° C. under a hydrogen
  2. customfor 30 hours
  3. concentrationThe reaction mixture was concentrated under reduced pressure of 20 mmHg
  4. customthe residue was purified by silica gel column chromatography
  5. additiona 7/3 (by volume) mixture of hexane and isopropanol as an eluent