HRID1272567
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
The fluticasone (4.66 kg) obtained as above is dissolved in mixture of methanol (45 lit) and dichloromethane (45 lit) under stirring at ambient temperature and charcoalized. The methylene chloride is recovered (by distillation) by distillation at atmospheric pressure. The mixture is then gradually cooled to 10° C. and stirred for 60 min. The crystallized product is filtered, washed with methanol (4.5 lit) and dried at 55–60° C. to obtain pure fluticasone propionate (Yield 4.09 kg, overall yield 84.51%, purity 99.37%).
WORKUP
后处理
- customThe methylene chloride is recovered
- distillation(by distillation)
- distillationby distillation at atmospheric pressure
- temperatureThe mixture is then gradually cooled to 10° C.
- stirringstirred for 60 min
- filtrationThe crystallized product is filtered
- washwashed with methanol (4.5 lit)
- customdried at 55–60° C.