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 solution of {[3-(4′,5′-difluoro-2′-methoxy-biphenyl-4-yloxymethyl)-benzoyl]-methyl-amino}-acetic acid ethyl ester (17 g, 36 mmol) in dioxane (400 mL) was treated with a solution of LiOH (4.4 g, 180 mmol) in water (400 mL) at room temperature for 12 h, followed by acidification with dilute HCl to pH-2-4. The mixture was extracted with ethyl acetate (3 times). The combined layer was washed with water and brine, dried over sodium sulfate, filtered, and evaporated to give {[3-(4′,5′-difluoro-2′-methoxy-biphenyl-4-yloxymethyl)-benzoyl]-methyl-amino}-acetic acid as an off-white solid, 13.5 g (85%), after drying in high vacuum at 60° C. for 48 h. LC-MS (ES) calculated for C26H25F2NO5, 441; found m/z 442 [M+H]+.
WORKUP
后处理
- extractionThe mixture was extracted with ethyl acetate (3 times)
- washThe combined layer was washed with water and brine
- dry with materialdried over sodium sulfate
- filtrationfiltered
- customevaporated