HRID1158944
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- filtrationThe product was filtered through a celite pad
- customevaporated
- customThe crude product thus obtained
- customwas purified by column chromatography on silica gel using
- additiona gradient mixture of ethyl acetate:hexane:methyl alcohol (7:7:1 to 4:4:1)