HRID1488859

反应详情

EQUATION

反应方程式

HRID 1488859 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

(E)-3-(3-Amino-4-methoxyphenyl)-2-(3,4,5-trimethoxyphenyl)-prop-2-enenitrile-Boc-L-prolineamide (1,250 mg, 2.33 mmols) was dissolved in 10 ml of dichloromethane, and 5 ml of a solution of 4-M hydrochloric acid and dioxane were added thereto. The mixture was reacted at room temperature for 1 hour. One-hundred milliliters of diethyl ether were added thereto, and the mixture was filtered. The resulting powder was purified through medium-pressure liquid chromatography (ODS, mixture of water and acetonitrile at a ratio of 70:30). The product was recrystallized three times with a mixture of chloroform and ethyl acetate at a ratio by volume of 1:10 to produce 465 mg (0.980 mmols) of the final product in a yield of 42%.

WORKUP

后处理

  1. customThe mixture was reacted at room temperature for 1 hour
  2. filtrationthe mixture was filtered
  3. customThe resulting powder was purified through medium-pressure liquid chromatography (
  4. additionODS, mixture of water and acetonitrile at a ratio of 70:30)
  5. customThe product was recrystallized three times
  6. additionwith a mixture of chloroform and ethyl acetate at a ratio by volume of 1:10