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