反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 2.5 °C
PROCEDURE
实验过程
Eprosartan acetate (30 gm, obtained in example 1) is suspended in acetone (450 ml) at 25-30° C., the suspension is cooled to 0-5° C., methanesulfonic acid (21.2 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 (60 ml) and stirred for 30 minutes at 25-30° C. The material is filtered, washed with acetone (30 ml) and then dried to give 29 gm of pure eprosartan mesylate [HPLC Purity: 99.95%; Specific Surface Area: 1.09 m2/g; Mean particle size (D50): 12.13 μm and 90 volume-% of the particles (D90): 33.48 μm].
WORKUP
后处理
- temperaturewhile maintaining the temperature at 0-5° C
- temperatureThe temperature of the mass is raised to 25-30° C.
- temperatureThe mass is cooled to 0-5° C.
- stirringstirred for 1 hour
- filtrationthe material is filtered
- customsuck dried
- additionTo the resulting wet cake is added acetone (60 ml)
- stirringstirred for 30 minutes at 25-30° C
- filtrationThe material is filtered
- washwashed with acetone (30 ml)
- customdried