HRID1665254

反应详情

EQUATION

反应方程式

HRID 1665254 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. extractionThe mixture was extracted with ethyl acetate (3 times)
  2. washThe combined layer was washed with water and brine
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. customevaporated