HRID420350

反应详情

EQUATION

反应方程式

HRID 420350 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
52.5 °C

PROCEDURE

实验过程

To a solution of 4-{3-[6-(3,5-di-pyridin-4-yl-phenoxy)-hexyl]-2-(2-ethoxycarbonyl-ethyl)-phenoxy}-butyric acid ethyl ester (195 mg, 0.3 mmol) in ethanol (10 mL) was added aqueous 1.0 N sodium hydroxide (8 mL) at room temperature. The mixture was heated to 50-55° C. and the resulting solution was stirred for 3 h. Then, the reaction mixture was concentrated and the residue was diluted with water (20 mL) and extracted with diethyl ether (50 mL) to remove any neutral impurities. The aqueous layer was acidified with 1 N hydrochloric acid until the solution become slightly acidic. The resulting white solids were collected by filtration and washed with water. After air-drying, 4-{2-(2-carboxy-ethyl)-3-[6-(3,5-di-pyridin-4-yl-phenoxy)-hexyl]-phenoxy}-butyric acid (176 mg, 99%) was isolated as a white solid: ES(+)-HRMS m/e calculated for C35H38N2O6 (M+H)+ 583.2803, found 584.2805.

WORKUP

后处理

  1. concentrationThen, the reaction mixture was concentrated
  2. additionthe residue was diluted with water (20 mL)
  3. extractionextracted with diethyl ether (50 mL)
  4. customto remove any neutral impurities
  5. filtrationThe resulting white solids were collected by filtration
  6. washwashed with water
  7. customAfter air-drying