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
To a solution of 200 mg of 2-[5-(2,4-Dichloro-phenyl)-2-methyl-6-(4-trifluoromethyl-phenyl)-pyridin-3-ylmethoxy]-2-methyl-propionic acid ethyl ester in 2 ml THF was added a solution of 18 mg of LiOH in 2 ml water at room temperature. After 16 h, the mixture was brought to pH 2 by addition of 1 M hydrochloric acid. The reaction mixture was concentrated under reduced pressure and the aqueous layer was extracted with dichloromethane. The combined organic phases were dried over MgSO4 and the solvents were removed under reduced pressure. The residue was purified by preparative HPLC (C18 reverse phase column, elution with a water/MeCN gradient with 0.1% TFA). The fractions containing the product were evaporated and lyophilized to yield a white solid. Yield: 22 mg.
WORKUP
后处理
- concentrationThe reaction mixture was concentrated under reduced pressure
- extractionthe aqueous layer was extracted with dichloromethane
- dry with materialThe combined organic phases were dried over MgSO4
- customthe solvents were removed under reduced pressure
- customThe residue was purified by preparative HPLC (
- washC18 reverse phase column, elution with a water/MeCN gradient with 0.1% TFA)
- additionThe fractions containing the product
- customwere evaporated
- customto yield a white solid