KR970703351A - Process for removing waste POx, alendronate and its by-products - Google Patents

Abstract

Removal of by-product phosphorus-containing substances (POx), allendronate and allendronate by-products, such as allendronate sodium, in the omera amino-1-hydroxy-C ₂ -C ₆ alkylidene-1,1-bisphosphonic acid synthesis process The method is described. First, calcium chloride is added to the crude liquor, calcium oxide is added to precipitate the POx material, and then the pH is neutralized to about 7 to complete the precipitation. Virtually all of the Alendronate sodium active ingredient is removed from the precipitate. Following filtration, the POx filter cake can be disposed of by landfilling, incineration or by regeneration as usable phosphorus fertilizer. The remaining filtrate can be further treated by recycling to wastewater treatment or process in an environmentally acceptable manner.

Description

Process for removing waste POx, alendronate and its by-products

[Brief Description of Drawings]

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Claims (10)

a) an aqueous medium consisting of salts of omega amino C ₂ -C ₆ alkylidene-1-hydroxy-1,1-bisphosphonic acid, metalsulfonic acid, phosphorous acid and phosphoric acid with calcium chloride as anhydrous salt relative to 100 parts by volume of the medium; Contacting with the calcium chloride compound in an amount of from about 10 parts by weight; b) contacting the solution of step (a) with calcium oxide in an amount sufficient to precipitate calcium / phosphorus containing salts; c) contacting the mixture of step (b) with an acid for adjusting the pH of the aqueous portion of the mixture to about 6 to 8 to precipitate calcium / phosphorous containing salts and d) precipitating the precipitate mixture of calcium / phosphorous containing salts from the aqueous medium. Separating. The compound of claim 1, wherein the omega amino C ₂ -C ₆ alkylidene-1,1-bisphosphonic acid is 4-amino-1-hydroxybutylidene-1,1-bisphosphonic acid, 2-amino-1- Hydroxyisobutylidene-1,1-bisphosphonic acid, 3-amino-1-hydroxypropylidene-1,1-bisphosphonic acid, 5-amino-1-hydroxypentylidene-1,1-bis Phosphonic acid and 6-amino-1-hydroxyhexylidene-1,1-bisphosphonic acid. The method of claim 2, wherein the omega amino C ₂ -C ₆ alkylidene-1,1-bisphosphonic acid is 4-amino-1-hydroxy-butylitrate-1,1-bisphosphonic acid. The process of claim 1 wherein the salts of omega amino C ₂ -C ₆ alkylidene-1-hydroxy-1,1-bisphosphonic acid, methanesulfonic acid, amine acid and phosphoric acid are sodium salts. The method of claim 1 wherein the calcium chloride compound is in hexahydrate form. The method of claim 1 wherein the calcium chloride is present in step (a) in an amount of from 2 to 7% w / v of the mother liquor. The method of claim 1 wherein the pH in step (b) is about 10-12. The process of claim 1 wherein the acid added in step (e) is hydrochloric acid. A precipitation mixture of calcium / phosphorus containing salts prepared by the method of claim 1. The precipitation mixture according to claim 9, which contains an alendronate. ※ Note: The disclosure is based on the initial application.