HRID1158944

反应详情

EQUATION

反应方程式

HRID 1158944 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The 3-(3-hydroxy-5-hydroxymethyl-2-methyl-pyridin-4-yl)-acrylic acid ethyl ester (34) (15.2 g, 64 mmol) in ethyl acetate (250 mL) was hydrogenated in the presence of 10% palladium on carbon (8.0 g) at room temperature overnight. The product was filtered through a celite pad and evaporated. The crude product thus obtained was purified by column chromatography on silica gel using a gradient mixture of ethyl acetate:hexane:methyl alcohol (7:7:1 to 4:4:1) to give 3-(3-hydroxy-5-hydroxymethyl-2-methyl-pyridin-4-yl)-propionic acid ethyl ester (35) (11.1 g, 62% yield) as a colorless solid.

WORKUP

后处理

  1. filtrationThe product was filtered through a celite pad
  2. customevaporated
  3. customThe crude product thus obtained
  4. customwas purified by column chromatography on silica gel using
  5. additiona gradient mixture of ethyl acetate:hexane:methyl alcohol (7:7:1 to 4:4:1)