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 mixture of {3-[2-(3-chlorobenzenesulfonyl)pyridin-3-ylmethyl]-5-fluoro-2-methylindol-1-yl}acetic acid methyl ester (0.10 g) and tetrahydrofuran (5.0 mL) was treated with 1.0 M aqueous lithium hydroxide solution (0.31 mL), and the resulting mixture was stirred at room temperature for 1 hour. The mixture was concentrated under reduced pressure and the pH adjusted to 4 by the addition of 0.1 M aqueous hydrochloric acid solution. The mixture was extracted with ethyl acetate and the combined extract was washed with saturated aqueous sodium chloride solution and dried over magnesium sulfate. The solvent was removed under reduced pressure and the residue purified by preparative reverse-phase HPLC, eluting with a mixture of acetonitrile and water (1:19 to 49:1 by volume) to afford the title compound as a white solid (0.085 g).
WORKUP
后处理
- concentrationThe mixture was concentrated under reduced pressure
- additionthe pH adjusted to 4 by the addition of 0.1 M aqueous hydrochloric acid solution
- extractionThe mixture was extracted with ethyl acetate
- extractionthe combined extract
- washwas washed with saturated aqueous sodium chloride solution
- dry with materialdried over magnesium sulfate
- customThe solvent was removed under reduced pressure
- customthe residue purified by preparative reverse-phase HPLC
- washeluting with a mixture of acetonitrile and water (1:19 to 49:1 by volume)