US2023301974A1PendingUtilityA1

Processes of making and crystalline forms of a mdm2 inhibitor

Assignee: AMGEN INCPriority: Jun 10, 2013Filed: May 8, 2023Published: Sep 28, 2023
Est. expiryJun 10, 2033(~6.9 yrs left)· nominal 20-yr term from priority
A61K 31/451C07D 211/94C07D 491/048C07C 309/25C07C 309/04C07C 313/02C07C 309/35C07D 498/04C07D 211/76C07B 2200/13A61K 31/45A61P 35/00A61P 43/00A61P 35/02
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Claims

Abstract

The present invention provides processes for making 2-((3R,5R,6S)-5-(3-chlorophenyl)-6-(4-chlorophenyl)-1-((S)-1-(isopropylsulfonyl)-3-methylbutan-2-yl)-3-methyl-2-oxopiperidin-3-yl)acetic acid as well as intermediates and processes for making the intermediates. Also provided are crystalline forms of the compound and the intermediates.

Claims

exact text as granted — not AI-modified
What is claimed is: 
     
         1 . Crystalline 
       
         
           
           
               
               
           
         
       
     
     
         2 . Crystalline anhydrous 
       
         
           
           
               
               
           
         
       
     
     
         3 . Crystalline anhydrous 
       
         
           
           
               
               
           
         
       
       characterized by a powder X-ray diffraction pattern comprising peaks at diffraction angle 2 theta degrees at approximately 11.6, 12.4, 18.6, 19.0, 21.6 and 23.6. 
     
     
         4 . Crystalline anhydrous 
       
         
           
           
               
               
           
         
       
       in accordance with  claim 3  having the X-ray diffraction pattern substantially shown in  FIG.  1   . 
     
     
         5 . A pharmaceutical composition comprising: crystalline 
       
         
           
           
               
               
           
         
       
       in accordance with  claims 2  or  3 ; and a pharmaceutically acceptable excipient. 
     
     
         6 . A method of treating bladder cancer, breast cancer, colon cancer, rectal cancer, kidney cancer, liver cancer, small cell lung cancer, non-small-cell lung cancer, esophagus cancer, gall-bladder cancer, ovarian cancer, pancreatic cancer, stomach cancer, cervix cancer, thyroid cancer, prostate cancer, squamous cell carcinoma, melanoma, acute lymphocytic leukemia, chronic myelogenous leukemia, acute lymphoblastic leukemia, B-cell lymphoma, T-cell-lymphoma, Hodgkin's lymphoma, non-Hodgkin's lymphoma, hairy cell lymphoma, Burkett's lymphoma, acute myelogenous leukemia, chronic myelogenous leukemia, endometrial cancer, head and neck cancer, glioblastoma, osteosarcoma, or rhabdomyosarcoma, the method comprising administering to a patient in need thereof, a therapeutically acceptable amount of a pharmaceutical composition comprising crystalline 
       
         
           
           
               
               
           
         
       
       in accordance with  claims 2  or  3 . 
     
     
         7 . The compound 
       
         
           
           
               
               
           
         
       
     
     
         8 . The compound 
       
         
           
           
               
               
           
         
       
     
     
         9 . Crystalline 
       
         
           
           
               
               
           
         
       
     
     
         10 . Crystalline 
       
         
           
           
               
               
           
         
       
       characterized by a powder X-ray diffraction pattern comprising peaks at diffraction angle 2 theta degrees at approximately 8.7, 18.5, 22.6 and 26.6. 
     
     
         11 . Crystalline 
       
         
           
           
               
               
           
         
       
       in accordance with  claim 10  having the X-ray diffraction pattern substantially shown in  FIG.  3   . 
     
     
         12 . The compound 
       
         
           
           
               
               
           
         
       
     
     
         13 . A process for making 
       
         
           
           
               
               
           
         
       
       the process comprising:
 reacting 
 
       
         
           
           
               
               
           
         
       
       under dehydrating conditions with, 
       
         
           
           
               
               
           
         
       
       to form 
       
         
           
           
               
               
           
         
       
     
     
         14 . The process of  claim 13  wherein the dehydrating conditions are azeotropic distillation with toluene. 
     
     
         15 . A process of making 
       
         
           
           
               
               
           
         
       
       the process comprising:
 reacting 
 
       
         
           
           
               
               
           
         
       
       with 
       
         
           
           
               
               
           
         
       
       to form 
       
         
           
           
               
               
           
         
       
       wherein X is CF 3 SO 3   −  or 
       
         
           
           
               
               
           
         
       
     
     
         16 . A process of making 
       
         
           
           
               
               
           
         
       
       the process comprising:
 reacting 
 
       
         
           
           
               
               
           
         
       
       with toluene to form 
       
         
           
           
               
               
           
         
       
     
     
         17 . A process of making 
       
         
           
           
               
               
           
         
       
       the process comprising:
 reacting 
 
       
         
           
           
               
               
           
         
       
       with lutidine and 
       
         
           
           
               
               
           
         
       
       to form 
       
         
           
           
               
               
           
         
       
     
     
         18 . A process of making 
       
         
           
           
               
               
           
         
       
       the process comprising reacting 
       
         
           
           
               
               
           
         
       
       with 
       
         
           
           
               
               
           
         
       
       to form 
       
         
           
           
               
               
           
         
       
       which is oxidized to 
       
         
           
           
               
               
           
         
       
       which is further converted to 
       
         
           
           
               
               
           
         
       
     
     
         19 . The process of  claim 18  wherein the oxidation is accomplished using ozone. 
     
     
         20 . The process of  claim 18  wherein the oxidation is accomplished using ozone followed by Pinnick oxidation. 
     
     
         21 . The process of  claim 18  wherein the conversion of 
       
         
           
           
               
               
           
         
       
       is accomplished using methanol and water. 
     
     
         22 . The process of  claim 18  wherein the oxidation is accomplished using ozone followed by Pinnick oxidation, and the conversion of 
       
         
           
           
               
               
           
         
       
       is accomplished using methanol and water. 
     
     
         23 . A process of making 
       
         
           
           
               
               
           
         
       
       the process comprising reacting 
       
         
           
           
               
               
           
         
       
       with 
       
         
           
           
               
               
           
         
       
       to form 
       
         
           
           
               
               
           
         
       
       oxidizing 
       
         
           
           
               
               
           
         
       
       to form 
       
         
           
           
               
               
           
         
       
       which is further converted to 
       
         
           
           
               
               
           
         
       
     
     
         24 . The process of  claim 23  wherein the 
       
         
           
           
               
               
           
         
       
       are reacted in the presence of a base. 
     
     
         25 . The process of  claim 24  wherein the base is sodium tert-butoxide. 
     
     
         26 . The process of  claim 23  wherein the oxidation is accomplished using RuCl 3  and NaIO 4 . 
     
     
         27 . The process of  claim 23  wherein the conversion of 
       
         
           
           
               
               
           
         
       
       is accomplished using methanol and water. 
     
     
         28 . The process of  claim 23  wherein the 
       
         
           
           
               
               
           
         
       
       are reacted in the presence of a base;
 the oxidation is accomplished using RuCl 3  and NaIO 4 ; and 
 the conversion of 
 
       
         
           
           
               
               
           
         
       
       is accomplished using methanol and water. 
     
     
         29 . The compound 
       
         
           
           
               
               
           
         
       
     
     
         30 . Crystalline 
       
         
           
           
               
               
           
         
       
     
     
         31 . Crystalline 
       
         
           
           
               
               
           
         
       
       characterized by a powder X-ray diffraction pattern comprising peaks at diffraction angle 2 theta degrees at approximately 10.5, 18.2, 20.3, 21, 21.9 and 24.2. 
     
     
         32 . Crystalline 
       
         
           
           
               
               
           
         
       
       in accordance with  claim 31  having the X-ray diffraction pattern substantially shown in  FIG.  6   . 
     
     
         33 . The compound 
       
         
           
           
               
               
           
         
       
     
     
         34 . Crystalline 
       
         
           
           
               
               
           
         
       
     
     
         35 . Crystalline 
       
         
           
           
               
               
           
         
       
       characterized by a powder X-ray diffraction pattern comprising peaks at diffraction angle 2 theta degrees at approximately 11.5, 14.3, 15.8, 17.7, 19.5 and 20.7. 
     
     
         36 . Crystalline 
       
         
           
           
               
               
           
         
       
       in accordance with  claim 35  having the X-ray diffraction pattern substantially shown in  FIG.  12   . 
     
     
         37 . A process of making 
       
         
           
           
               
               
           
         
       
       the process comprising reacting 
       
         
           
           
               
               
           
         
       
       with an oxidizing agent and DABCO to form 
       
         
           
           
               
               
           
         
       
       and reacting 
       
         
           
           
               
               
           
         
       
       with an acid to form 
       
         
           
           
               
               
           
         
       
     
     
         38 . The process of  claim 37  wherein the oxidizing agent is ozone and the acid is hydrochloric acid.

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