Water → Alendronate Sodium
Reaction equation
[CH2:1]([CH2:13][NH2:14])[CH2:2][C:3]([P:9]([O-:12])([OH:11])=[O:10])([P:5]([OH:8])([OH:7])=[O:6])[OH:4].[Na+:15].[OH2:16]>C(C(C)=O)C>[CH2:1]([CH2:13][NH2:14])[CH2:2][C:3]([P:5]([O-:7])([OH:8])=[O:6])([P:9]([OH:12])([OH:11])=[O:10])[OH:4].[OH2:16].[OH2:4].[OH2:4].[Na+:15]Participants
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 72 °C
Procedure
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
- 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
Sources & evidence
- ORD record
- ord-f62ea877f81e4aeca05b9c435f19569d
- Source dataset
- uspto-grants-2011_08
- Patent number
- US08003820B2
Reaction notes
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