HRID2261808
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
A suspension of 5-butoxy-isophthalic acid dimethyl ester (2.0 g, 7.5 mmol) in THF/MeOH/water (5.0 mL each) is treated with lithium hydroxide (0.22 g, 9.0 mmol) at room temperature for 1.0 h. The reaction mixture is acidified with 1.0 M HCl and the product is extracted with EtOAc (30 mL), washed with brine (30 mL), dried (Na2SO4), filtered, and concentrated under reduced pressure to a residue. The residue is purified by flash chromatography to afford the title compound as solid (1.0 g, 53%). LC-ES/MS m/e 270.3 (M+18), 251.3 (M−1).
WORKUP
后处理
- extractionthe product is extracted with EtOAc (30 mL)
- washwashed with brine (30 mL)
- dry with materialdried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated under reduced pressure to a residue
- customThe residue is purified by flash chromatography