HRID1676015

反应详情

EQUATION

反应方程式

HRID 1676015 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customA clear solution was prepared
  2. temperatureby heating
  3. filtrationthan filtered through cloth
  4. washthe filter was washed with 8 ml of water
  5. customthe filtrate was transferred into another round bottom flask
  6. temperatureto cooling to a temperature of about 30° C. and than to 5° C.
  7. stirringwith simultaneous stirring for a period of about 90 minutes until the solid
  8. customseparated
  9. customThe solid that was obtained
  10. customwas separated through filtration
  11. washby washing with a mixture of 2 ml of methyl ethyl ketone and 4 ml of water
  12. customdrying at a temperature of about 25° C. for a period of about 20 minutes
  13. customto drying in an oven