US2004029813A1PendingUtilityA1

Novel $g(beta crystalline form of perindopril tert-butylamine salt, preparation method, and pharmaceutical compositions containing same

Priority: Jul 6, 2000Filed: Jul 6, 2001Published: Feb 12, 2004
Est. expiryJul 6, 2020(expired)· nominal 20-yr term from priority
A61P 9/00A61P 9/12A61P 9/10A61P 9/04A61P 43/00A61P 7/10A61P 13/02C07D 209/42A61K 31/404
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Claims

Abstract

β crystalline form of the compound of formula (I): characterised by its powder X-ray diffraction diagram. Medicaments.

Claims

exact text as granted — not AI-modified
1 . β Crystalline Form of the Compound of Formula (I):  
       
         
           
           
               
               
           
         
       
       characterised by the following powder x-ray diffraction diagram measured using a diffractometer (copper anticathode) and expressed in terms of inter-planar distance d, Bragg's angle 2 theta, intensity and relative intensity (expressed as a percentage with respect to the most intense ray):  
       
         
           
                 
                 
                 
                 
               
                     
                 
                     
                 
                   Angle 2 theta 
                   Inter-planar 
                     
                   Relative intensity 
                 
                   (°) 
                   distance d (Å) 
                   Intensity 
                   (%) 
                 
                     
                 
                     
                 
                 
                 
                 
                 
               
                   5.169 
                   17.08 
                   523 
                   16.5 
                 
                   8.379 
                   10.54 
                   1001 
                   31.5 
                 
                   9.350 
                   9.45 
                   3175 
                   100 
                 
                   14.746 
                   6.00 
                   236 
                   7.4 
                 
                   15.411 
                   5.74 
                   753 
                   23.7 
                 
                   15.931 
                   5.56 
                   279 
                   8.8 
                 
                   16.711 
                   5.30 
                   113 
                   3.6 
                 
                   18.161 
                   4.88 
                   122 
                   3.8 
                 
                   20.564 
                   4.32 
                   1198 
                   37.7 
                 
                   21.285 
                   4.17 
                   330 
                   10.4 
                 
                   21.781 
                   4.08 
                   317 
                   10 
                 
                   22.632 
                   3.93 
                   190 
                   6 
                 
                   23.308 
                   3.81 
                   133 
                   4.2 
                 
                   23.797 
                   3.74 
                   427 
                   13.4 
                 
                   24.276 
                   3.66 
                   118 
                   3.7 
                 
                   25.190 
                   3.53 
                   92 
                   2.9 
                 
                   25.924 
                   3.43 
                   251 
                   7.9 
                 
                   26.646 
                   3.34 
                   250 
                   7.9 
                 
                   27.620 
                   3.23 
                   96 
                   3 
                 
                   28.306 
                   3.15 
                   133 
                   4.2 
                 
                     
                 
                     
                 
             
                
                
                
                
                
               
               
                
               
            
             
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
               
            
           
         
       
     
     
         2 . Process for the preparation of the β crystalline form of the compound of formula (1) according to  claim 1 , characterised in that a solution of perindopril tert-butylamine salt in dichloromethane is heated at reflux, the solution is then cooled to 0° C. and the solid obtained is collected by filtration.  
     
     
         3 . Process for the preparation of the β crystalline form of the compound of formula (I) according to  claim 1 , characterised in that a solution of perindopril tert-butylamine salt in ethyl acetate is heated at reflux, the solution is rapidly cooled to 5° C. and the solid obtained is then collected by filtration.  
     
     
         4 . Process according to either  claim 2  or  claim 3 , characterised in tat the compound of formula (I) obtained by the preparation process described in patent specification EP 0 308 341 is used.  
     
     
         5 . Process according to  claim 2 , characterised in that the concentration of the compound of formula (I) in the dichloromethane is from 100 to 200 g/litre.  
     
     
         6 . Process according to  claim 3 , characterised in that the concentration of the compound of formula (I) in the ethyl acetate is from 70 to 90 g/litre.  
     
     
         7 . Pharmaceutical composition comprising as active ingredient the compound according to  claim 1 , in combination with one or more pharmaceutically acceptable, inert, non-toxic carriers.  
     
     
         8 . Pharmaceutical composition according to  claim 7  for use in the manufacture of medicaments for use as inhibitors of angiotensin I converting enzyme.  
     
     
         9 . Pharmaceutical composition according to  claim 8  for use in the manufacture of medicaments for use in the treatment of cardiovascular diseases.  
     
     
         10 . Pharmaceutical composition according to any one of  claims 7  to  9 , characterised in that it also comprises a diuretic.  
     
     
         11 . Pharmaceutical composition according to  claim 10 , characterised in tat the diuretic is indapamide.

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