HRID1808669

反应详情

EQUATION

反应方程式

HRID 1808669 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

Eprosartan free base (8 gm, obtained in example 3) is suspended in acetone (120 ml) at 25-30° C., the suspension is cooled to 0-5° C., methanesulfonic acid (5.4 gm) is added drop wise while maintaining the temperature at 0-5° C. The temperature of the mass is raised to 25-30° C. and stirred for 5 hours. The mass is cooled to 0-5° C., stirred for 1 hour, the material is filtered and then suck dried. To the resulting wet cake is added acetone (16 ml) and stirred for 15 minutes at 25-30° C. The material is filtered, washed with acetone (8 ml) and then dried to give 9 gm of pure eprosartan mesylate [HPLC Purity: 99.96%; Specific Surface Area: 1.11 m2/g; Mean particle size (D50): 11.23 μm and 90 volume-% of the particles (D90): 30.42 μm].

WORKUP

后处理

  1. temperaturewhile maintaining the temperature at 0-5° C
  2. temperatureThe temperature of the mass is raised to 25-30° C.
  3. temperatureThe mass is cooled to 0-5° C.
  4. stirringstirred for 1 hour
  5. filtrationthe material is filtered
  6. customsuck dried
  7. additionTo the resulting wet cake is added acetone (16 ml)
  8. stirringstirred for 15 minutes at 25-30° C
  9. filtrationThe material is filtered
  10. washwashed with acetone (8 ml)
  11. customdried