HRID41055

反应详情

EQUATION

反应方程式

HRID 41055 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of (+/−)-3-(5-ethoxy-1H-indol-3-yl)-2-methyl-2-nitro-propionic acid methyl ester (5.3 g, 17.3 mmol) in dry methanol (50 ml) Raney nickel is added and the mixture is stirred at room temperature under H2 at atmospheric pressure overnight. The reaction mixture is filtered through a pad of Celite and the solid is washed with methanol. The filtrate is concentrated and the residue is purified by column chromatography (dichloromethane-methanol, 95:5) to give (+/−)-2-amino-3-(5-ethoxy-1H-indol-3-yl)-2-methyl-propionic acid methyl ester (4.2 g, 90%) as a white crystals. M.p. 165-166° C. (from ethyl acetate-hexane).

WORKUP

后处理

  1. filtrationThe reaction mixture is filtered through a pad of Celite
  2. washthe solid is washed with methanol
  3. concentrationThe filtrate is concentrated
  4. customthe residue is purified by column chromatography (dichloromethane-methanol, 95:5)