HRID2089633

反应详情

EQUATION

反应方程式

HRID 2089633 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
45 °C

PROCEDURE

实验过程

To a mixture of [1-amino-1-[4-({(5-chloromethoxy-1-pyrimidin-2-yl-1H-[1,2,4]triazol-3-yl)-[2-fluoro-3-(2-hydroxyethoxy)-5-methoxyphenyl]methyl}amino)phenyl]methylidene]carbamic acid 2,2-dimethylpropyl ester (Example 2b, 100 mg), potassium hydrogen carbonate (109 mg), and DMF (13.3 mL), 2-ethylbutanoic acid (88.3 mg) and sodium iodide (117 mg) were added, and the resulting mixture was stirred at 45° C. overnight and then cooled to room temperature. To the reaction mixture, ice and saturated aqueous ammonium chloride solution were added, and the resulting mixture was extracted with a mixture of THF and ethyl acetate. The organic layer was washed with saturated aqueous ammonium chloride solution and dried over anhydrous magnesium sulfate.

WORKUP

后处理

  1. additionwere added
  2. temperaturecooled to room temperature
  3. extractionthe resulting mixture was extracted with a mixture of THF and ethyl acetate
  4. washThe organic layer was washed with saturated aqueous ammonium chloride solution
  5. dry with materialdried over anhydrous magnesium sulfate