HRID355528

反应详情

EQUATION

反应方程式

HRID 355528 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6 g of sodium acetate trihydrate are dissolved in 20 ml of water. 40 ml of acetone and 20 g of cefotaxime in free acid form are added to the stirred solution. The mixture is cooled to 0°. A solution is obtained within 2 to 5 minutes. The solution is filtered through a filter bed and subsequently through a sterile filter. The filters are washed with a chilled mixture of 3 ml of water and 15 ml of acetone. The filtrate is seeded with 0.2 g of seed crystals (Claforan®) and warmed to 20°. The mixture is stirred for 60 minutes. The sodium salt of cefotaxime partially crystallises. In order to compete crystallisation, 300 ml of acetone are added dropwise within 3 hours, and stirring is effected for a further 30 minutes at 20°. The sodium salt of cefotaxime is separated off by filtration, washed with acetone and dried overnight in a vacuum drying chamber at 40° and for 1.5 hours in a stream of dry nitrogen gas at 70°. Crystalline sodium cefotaxime substantially in form of needles is obtained.

WORKUP

后处理

  1. temperatureThe mixture is cooled to 0°
  2. customA solution is obtained within 2 to 5 minutes
  3. filtrationThe solution is filtered through a filter bed and subsequently through a sterile filter
  4. washThe filters are washed with a chilled mixture of 3 ml of water and 15 ml of acetone
  5. temperaturewarmed to 20°
  6. customThe sodium salt of cefotaxime partially crystallises
  7. customcrystallisation, 300 ml of acetone
  8. additionare added dropwise within 3 hours
  9. stirringstirring
  10. waitis effected for a further 30 minutes at 20°
  11. customThe sodium salt of cefotaxime is separated off by filtration
  12. washwashed with acetone
  13. customdried overnight in a vacuum
  14. customdrying chamber at 40°
  15. waitfor 1.5 hours in a stream of dry nitrogen gas at 70°