HRID891027

反应详情

EQUATION

反应方程式

HRID 891027 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

The pH was raised to 8.5 by addition of 2M sodium hydroxide in water (1.2 ml) and the solution was heated to 50° C. Acetonitrile (90 ml) was added to the mixture and then the mixture was stirred at elevated temperature for one hour. The mixture was allowed to cool to 20–25° C. (“ambient temperature”), was held at ambient temperature for two hours and then cooled to 5° C. and maintained at 5° C. for 12 hours, whereupon pravastatin sodium crystallized. The crystals were then isolated by filtration and washed with acetonitrile (2×10 ml) and dried under vacuum at 50° C. X-ray diffraction analysis revealed the presence of Form A. Pravastatin Form A was obtained in 92% yield.

WORKUP

后处理

  1. temperatureto cool to 20–25° C. (“ambient temperature”)
  2. waitwas held at ambient temperature for two hours
  3. temperaturecooled to 5° C.
  4. customcrystallized
  5. customThe crystals were then isolated by filtration
  6. washwashed with acetonitrile (2×10 ml)
  7. customdried under vacuum at 50° C