HRID1843718

反应详情

EQUATION

反应方程式

HRID 1843718 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Methyl 3-[2-({4-[(2-methoxypyridin-4-yl)oxy]-2-(methylamino)phenyl}amino)-2-oxoethoxy]benzoate produced in Example (16e) (4.52 g, 10.3 mmol) and acetic acid (50 mL) was stirred at 80° C. for two hours. The reaction mixture was concentrated and then water (100 mL) and sodium bicarbonate were added, followed by extraction with ethyl acetate (100 mL). The organic layer was washed with a saturated sodium bicarbonate aqueous solution (100 mL) twice and dried over anhydrous sodium sulfate. After concentration under reduced pressure, the residue was purified by silica gel chromatography (hexane/ethyl acetate, 1:1) to obtain the title compound (3.10 g, 72%) as a white solid.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated
  2. additionwater (100 mL) and sodium bicarbonate were added
  3. extractionfollowed by extraction with ethyl acetate (100 mL)
  4. washThe organic layer was washed with a saturated sodium bicarbonate aqueous solution (100 mL) twice
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationAfter concentration under reduced pressure
  7. customthe residue was purified by silica gel chromatography (hexane/ethyl acetate, 1:1)