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
- 72 °C
PROCEDURE
实验过程
A clear solution was prepared by dissolving 20 g of crude alendronate sodium in a solvent mixture containing 400 ml of water and 100 ml of methyl ethyl ketone by heating to reflux at temperature of about 72° C. with simultaneous stirring over a period of about 70 minutes. The solution was than filtered through cloth to make it free from particles, the filter was washed with 8 ml of water and the filtrate was transferred into another round bottom flask, subjected to cooling to a temperature of about 30° C. and than to 5° C. with simultaneous stirring for a period of about 90 minutes until the solid separated. The solid that was obtained was separated through filtration followed by washing with a mixture of 2 ml of methyl ethyl ketone and 4 ml of water and subjected to suction drying at a temperature of about 25° C. for a period of about 20 minutes. Then the obtained wet solid was finally subjected to drying in an oven by applying vacuum at about 100 millibarto afford 17 g (yield 85%) alendronate sodium trihydrate.
WORKUP
后处理
- customA clear solution was prepared
- temperatureby heating
- filtrationthan filtered through cloth
- washthe filter was washed with 8 ml of water
- customthe filtrate was transferred into another round bottom flask
- temperatureto cooling to a temperature of about 30° C. and than to 5° C.
- stirringwith simultaneous stirring for a period of about 90 minutes until the solid
- customseparated
- customThe solid that was obtained
- customwas separated through filtration
- washby washing with a mixture of 2 ml of methyl ethyl ketone and 4 ml of water
- customdrying at a temperature of about 25° C. for a period of about 20 minutes
- customto drying in an oven