HRID525309

反应详情

EQUATION

反应方程式

HRID 525309 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-2.5 °C

PROCEDURE

实验过程

The crude abiraterone thus obtained (about 64 g) is taken up in methylene chloride (350 mL), and the resulting mixture, cooled to a temperature of −5 to 0° C., is added with acetic anhydride (130 mL) and then with triethylamine (190 mL), maintaining the temperature at −5 to 0° C. The mixture is stirred at room temperature for about 25 h, then washed with water and concentrated under vacuum, taking up the residue in acetone (250 mL). The resulting solid is isolated by filtration (at 0-5° C.) and dried under vacuum at 40° C. for 16 h (about 46 g; purity: 82.5%; assay: about 73%). A second fraction of crude abiraterone acetate, as an oil, is obtained by concentration of the mother liquor under vacuum (54 g, purity: 74%, assay: about 45%).

WORKUP

后处理

  1. washwashed with water
  2. concentrationconcentrated under vacuum
  3. customThe resulting solid is isolated by filtration (at 0-5° C.)
  4. customdried under vacuum at 40° C. for 16 h (about 46 g; purity: 82.5%; assay: about 73%)