HRID41054

反应详情

EQUATION

反应方程式

HRID 41054 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of (+/−)-3-(5-methoxy-1H-indol-3-yl)-2-methyl-2-nitro-propionic acid methyl ester (4.26 g) in methanol (80 mL) wet Raney nickel (ca 12 g) is added, and the mixture is stirred under hydrogen at atmospheric pressure at room temperature overnight. The solid is filtered through Celite, is washed with methanol, and the filtrate is concentrated. Column chromatography of the residue (dichloromethane-methanol, 98:2→95:5) gives the title compound (3.45 g, 90%). M.p. 131-132° C. (from ethyl acetate-light petroleum).

WORKUP

后处理

  1. filtrationThe solid is filtered through Celite
  2. washis washed with methanol
  3. concentrationthe filtrate is concentrated