HRID1427015

反应详情

EQUATION

反应方程式

HRID 1427015 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
75 °C

PROCEDURE

实验过程

N-(4-((6-ethoxy-1H-indol-5-yl)oxy)pyridin-2-yl)acetamide described in Production Example 15-5 (7.16 g, 23.0 mmol) was dissolved in methanol (50 mL), a 2 M sodium hydroxide solution (50 mL) was added under nitrogen atmosphere at room temperature, and the mixture was heated and stirred at 75° C. for 2.5 hours. The reaction mixture was cooled to room temperature and then water and ethyl acetate were added for partition. The aqueous layer was extracted with ethyl acetate and the combined organic layer was washed with a saturated saline solution. The organic layer was dried over anhydrous magnesium sulfate, then the resultant was filtered and concentrated under vacuum. A liquid mixture of diethyl ether and ethyl acetate was added to the residue, and the mixture was collected by filteration and washed to obtain the title compound (5.35 g, 86%).

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureThe reaction mixture was cooled to room temperature
  3. customfor partition
  4. extractionThe aqueous layer was extracted with ethyl acetate
  5. washthe combined organic layer was washed with a saturated saline solution
  6. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  7. filtrationthe resultant was filtered
  8. concentrationconcentrated under vacuum
  9. additionA liquid mixture of diethyl ether and ethyl acetate
  10. additionwas added to the residue
  11. customthe mixture was collected by filteration
  12. washwashed