Production of agglomerates

Abstract

A process for producing spherical agglomerates of inogatran having a narrow size distribution, and the compound inogatran anhydrate.

1 . A process for producing spherical agglomerates of inogatran comprising the consecutive steps of: 
 a) dissolving inogatran in one of its instable, hygroscopic, hydrate forms in a mixture of a good solvent for inogatran (L1) and a poor solvent for inogatran (L3) to form a concentrated solution,    b) optionally filtering the solution,    c) concentrating the concentrated solution further,    d) adding a non-solvent for inogatran (L2) to obtain supersaturation, and    e) adding further (L2) when nucleation has started.    
     
     
         2 . A process according to  claim 1 , wherein the obtained product is worked up.  
     
     
         3 . A process according to  claim 1 , wherein the mixture of (L1) and (L3) has a ratio in the range 0.97-0.90:0.03-0.10 (w/w).  
     
     
         4 . A process according to  claim 1 , wherein the amount of (L1), (L2) and (L3) per weight of inogatran is in the range from 7 to 15 ml per g inogatran.  
     
     
         5 . A process according to  claim 1 , wherein the ratio of [(L1)+(L3)]:L2) is from 1:1.5 to 1:4 (v/v).  
     
     
         6 . A process according to  claim 1 , wherein in step a) a concentrated solution is a solution having more than 10 g inogatran per 100 ml of solvent, preferably more than 20 g inogatran per 100 ml of solvent.  
     
     
         7 . A process according to any one of the preceding claims wherein L1 is ethanol.  
     
     
         8 . A process according to any one of the preceding claims wherein L2 is ethyl acetate.  
     
     
         9 . A process according to any one of the preceding claims wherein L3 is water.  
     
     
         10 . Inogatran anhydrate.