US2007232798A1PendingUtilityA1

Process For The Synthesis Of 2'-O-Substituted Pyrimidines And Oligomeric Compounds Therefrom

Individually held — no corporate assignee on recordPriority: Mar 6, 1995Filed: Mar 12, 2007Published: Oct 4, 2007
Est. expiryMar 6, 2015(expired)· nominal 20-yr term from priority
Y02P20/55C07H 21/00A61P 35/00Y02P20/582A61P 37/04A61P 31/18C07H 19/06A61P 31/12
57
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Claims

Abstract

Oligonucleotide analogs are disclosed having pyrimidine monomeric sub-units therein that are modified at the 2′ and 5′ positions. Monomeric sub-units having these modifications may be further modified at the 2′ position. Improved processes for the synthesis of 2′-O-substituted pyrimidine nucleosides are also provided. The processes feature alkylation of a 2,2′-anhydropyrimidine nucleoside or a 2S,2′-anhydropyrimidine nucleoside with a weak nucleophile in the presence of a Lewis acid.

Claims

exact text as granted — not AI-modified
1 . An oligomeric compound comprising at least one monomeric sub-unit of structure I:  
       
         
           
           
               
               
           
         
       
       wherein: 
 X is hydroxyl or amino;  
 R is halo or C 1 -C 6  alkyl or substituted C 1 -C 6  alkyl wherein said substitution is halo, amino, hydroxyl, thiol, ether or thioether;  
 L is oxygen or sulfur;  
 Z is fluoro or O—R 1 X 1 , where R 1  is C 1 -C 6  alkyl, C 6 -C 10  aryl, C 7 -C 18  alkaryl and X 1  is H, NH 2  or imidazole; and  
 one of Q 1  and Q 2  is attached via a linking moiety to a nucleotide, oligonucleotide, nucleoside, or oligonucleoside and the other of said Q 1  and Q 2 , is a hydroxyl, a protected hydroxyl, an activated solid support, a nucleotide, an oligonucleotide, a nucleoside, an oligonucleoside, an oligo-nucleotide/nucleoside, an activated phosphate, a phosphate, an activated phosphite, or a phosphite.  
 
     
     
         2 . The oligomeric compound of  claim 1 , wherein L is O.  
     
     
         3 . The oligomeric compound of  claim 1 , wherein Z is F.  
     
     
         4 . The oligomeric compound of  claim 1 , comprising from 5 to 200 sub-units.  
     
     
         5 . The oligomeric compound of  claim 1 , comprising from 5 to 50 sub-units.  
     
     
         6 . The oligomeric compound of  claim 1 , comprising from 10 to 20 sub-units.  
     
     
         7 . The oligomeric compound of  claim 1 , wherein said linking moiety comprises a phosphodiester, phosphotriester, hydrogen phosphonate, alkylphosphonate, alkylphosphonothioate, arylphosphonothioate, phosphorothioate, phosphorodithioate, or phosphoramidate.  
     
     
         8 . The oligomeric compound of  claim 1  having a plurality of monomeric sub-units of structure I.  
     
     
         9 . The oligomeric compound of  claim 8  wherein said monomeric sub-units are located at preselected positions.  
     
     
         10 . An oligomeric compound comprising at least one monomeric sub-unit of structure II:  
       
         
           
           
               
               
           
         
       
       wherein: 
 X is hydroxyl or amino;  
 R is halo or C 1 -C 6  alkyl or substituted C 1 -C 6  alkyl wherein said substitution is halo, amino, hydroxyl, thiol, ether or thioether;  
 L is oxygen or sulfur; and  
 one of Q 1  and Q 2  is attached via a linking moiety to a nucleotide, oligonucleotide, nucleoside, or oligonucleoside and the other of said Q 1  and Q 2 , is a hydroxyl, a protected hydroxyl, an activated solid support, a nucleotide, an oligonucleotide, a nucleoside, an oligonucleoside, an oligo-nucleotide/nucleoside, an activated phosphate, a phosphate, an activated phosphite, or a phosphite.  
 
     
     
         11 . The oligomeric compound of  claim 10 , wherein L is O.  
     
     
         12 . The oligomeric compound of  claim 10 , comprising from 5 to 50 sub-units.  
     
     
         13 . The oligomeric compound of  claim 10 , comprising from 10 to 20 sub-units.  
     
     
         14 . The oligomeric compound of  claim 10 , wherein said linking moiety comprises a phosphodiester, phosphotriester, hydrogen phosphonate, alkylphosphonate, alkylphosphonothioate, arylphosphonothioate, phosphorothioate, phosphorodithioate, or phosphoramidate.  
     
     
         15 . The oligomeric compound of  claim 10  having a plurality of monomeric sub-units of structure II.  
     
     
         16 . The oligomeric compound of  claim 15  wherein said monomeric sub-units are located at preselected positions.  
     
     
         17 . An oligomeric compound comprising at least one monomeric sub-unit of structure III:  
       
         
           
           
               
               
           
         
       
       wherein: 
 X is hydroxyl or amino;  
 R is halo or C 1 -C 6  alkyl or substituted C 1 -C 6  alkyl wherein said substitution is halo, amino, hydroxyl, thiol, ether or thioether;  
 L is oxygen or sulfur;  
 R 1  is C 1 -C 6  alkyl, C 6 -C 10  aryl, C 7 -C 18  alkaryl and X 1  is H, NH 2  or imidazole; and  
 one of Q 1  and Q 2  is attached via a linking moiety to a nucleotide, oligonucleotide, nucleoside, or oligonucleoside and the other of said Q 1  and Q 2 , is a hydroxyl, a protected hydroxyl, an activated solid support, a nucleotide, an oligonucleotide, a nucleoside, an oligonucleoside, an oligo-nucleotide/nucleoside, an activated phosphate, a phosphate, an activated phosphite, or a phosphite.  
 
     
     
         18 . The oligomeric compound of  claim 17 , wherein L is O.  
     
     
         19 . The oligomeric compound of  claim 17 , comprising from 5 to 50 sub-units.  
     
     
         20 . The oligomeric compound of  claim 17 , comprising from 5 to 50 sub-units.  
     
     
         21 . The oligomeric compound of  claim 17 , wherein said linking moiety comprises a phosphodiester, phosphotriester, hydrogen phosphonate, alkylphosphonate, alkylphosphonothioate, arylphosphonothioate, phosphorothioate, phosphorodithioate, or phosphoramidate.  
     
     
         22 . The oligomeric compound of  claim 17  having a plurality of monomeric sub-units of structure I.  
     
     
         23 . The oligomeric compound of  claim 22  wherein said monomeric sub-units are located at preselected positions.  
     
     
         24 . A process for the synthesis of a 2′-O-substituted pyrimidine nucleoside of formula:  
       
         
           
           
               
               
           
         
       
       wherein: 
 Q is a pyrimidine base or a 2-S pyrimidine base;  
 R 1  is substituted or unsubstituted C 1 -C 30  alkyl, C 1 -C 30  alkenyl, C 1 -C 30  alkynyl, C 6 -C 14  aryl, or C 7 -C 30  aralkyl, wherein said substitution is halo, amino, hydroxyl, thiol, ether or thioether; and  
 R 2  and R 3  are independently hydrogen or a hydroxyl protecting group;  
 comprising the steps of:  
 providing a 2-2′-anhydropyrimidine nucleoside;  
 selecting an alcohol of the formula R 1 —OH; and  
 treating said 2-2′-anhydropyrimidine nucleoside and said alcohol with a Lewis acid under conditions of time, temperature and pressure effective to yield said 2′-O-substituted pyrimidine nucleoside.  
 
     
     
         25 . The process of  claim 24  wherein said 2-2′-anhydropyrimidine nucleoside and said alcohol are treated in a pressure sealed vessel.  
     
     
         26 . The process of  claim 24  wherein said Lewis acid is a borate.  
     
     
         27 . The process of  claim 26  wherein said borate is a trialkyl borate.  
     
     
         28 . The process of  claim 27  wherein the formula of said trialkyl borate is B(OR 1 ) 3 .  
     
     
         29 . The process of  claim 28  wherein said trialkyl borate is prepared from the treatment of borane with an alcohol.  
     
     
         30 . The process of  claim 29  wherein said trialkyl borate is prepared from the treatment of borane with an alcohol of formula HO—R 1 .  
     
     
         31 . The process of  claim 24  wherein R 1  is C 1 -C 10  alkyl.  
     
     
         32 . The process of  claim 24  wherein R 1  is C 6 -C 14  aryl.  
     
     
         33 . The process of  claim 24  wherein said treating comprises heating at from about 120° C. to about 200° C.  
     
     
         34 . The process of  claim 24  wherein said pyrimidine nucleoside is uridine or 5-methyluridine.  
     
     
         35 . A process for the synthesis of a 2′-O-substituted cytidine nucleoside of formula:  
       
         
           
           
               
               
           
         
       
       wherein: 
 X′ is O or S;  
 R 1  is substituted or unsubstituted C 1 -C 30  alkyl, C 1 -C 30  alkenyl, C 1 -C 30  alkynyl, C 6 -C 14  aryl, or C 7 -C 30  aralkyl, wherein said substitution is halo, amino, hydroxyl, thiol, ether or thioether;  
 R 2  and R 3  are independently hydrogen or a hydroxyl protecting group;  
 R 5  and R 6  are independently H, C 1 -C 30  hydrocarbyl or substituted C 1 -C 30  hydrocarbyl;  
 comprising the steps of:  
 providing a 2-2′-anhydrouridine nucleoside of formula:  
                     
 selecting an alcohol of formula R 1 —OH;  
 treating said 2-2′-anhydrouridine nucleoside and said alcohol with a Lewis acid under conditions of time, temperature and pressure effective to form a 2′—O— substituted uridine nucleoside; and  
 aminating said 2′-O-substituted uridine nucleoside to said 2′-O-substituted cytidine nucleoside.  
 
     
     
         36 . The process of  claim 35  wherein said 2-2′-anhydrouridine nucleoside and said alcohol are treated in a pressure sealed vessel.  
     
     
         37 . The process of  claim 35  wherein said Lewis acid is a borate.  
     
     
         38 . The process of  claim 37  wherein said borate is a trialkyl borate.  
     
     
         39 . The process of  claim 38  wherein the formula of said trialkyl borate is B(OR 1 ) 3 .  
     
     
         40 . The process of  claim 38  wherein said trialkyl borate is prepared from the treatment of borane with an alcohol.  
     
     
         41 . The process of  claim 40  wherein said trialkyl borate is prepared from the treatment of borane with an alcohol of formula HO—R 1 .  
     
     
         42 . The process of  claim 35  wherein R 1  is C 1 -C 10  alkyl.  
     
     
         43 . The process of  claim 35  wherein R 1  is C 6 -C 14  aryl.  
     
     
         44 . The process of  claim 35  wherein said treating comprises heating from about 120° C. to about 200° C.  
     
     
         45 . The process of  claim 35  wherein said 2′-O-substituted cytidine nucleoside is 2′-O-methyl-S-methylcytidine.  
     
     
         46 . An oligomeric compound comprising at least one monomeric sub-unit of formula:  
       
         
           
           
               
               
           
         
       
       wherein: 
 A is hydroxyl or amino;  
 R is halo or C 1 -C 6  alkyl or substituted C 1 -C 6  alkyl wherein said substitution is halo, amino, hydroxyl, thiol, ether or thioether;  
 L is oxygen or sulfur;  
 Z′ is substituted or unsubstituted C 1 -C 30  alkyl, C 1 -C 30  alkenyl, C 1 -C 30  alkynyl, C 6 -C 14  aryl, or C 7 -C 30  aralkyl, wherein said substitution is halo, amino, hydroxyl, thiol, ether or thioether; and  
 one of Q 1  and Q 2  is attached via a linking moiety to a nucleotide, oligonucleotide, nucleoside, or oligonucleoside and the other of said Q 1  and Q 2 , is a hydroxyl, a protected hydroxyl, an activated solid support, a nucleotide, an oligonucleotide, a nucleoside, an oligonucleoside, an oligo-nucleotide/nucleoside, an activated phosphate, a phosphate, an activated phosphite, or a phosphite.  
 
     
     
         47 . The oligomeric compound of  claim 46 , wherein L is O.  
     
     
         48 . The oligomeric compound of  claim 46 , wherein Z is —(CH 2 ) n —O—(CH 2 ) n —CH 3 .  
     
     
         49 . The oligomeric compound of  claim 48 , wherein n is 2 and m is 0.  
     
     
         50 . The oligomeric compound of  claim 46 , comprising from 5 to 200 sub-units.  
     
     
         51 . The oligomeric compound of  claim 46 , comprising from 5 to 50 sub-units.  
     
     
         52 . The oligomeric compound of  claim 46 , comprising from 10 to 20 sub-units.  
     
     
         53 . The oligomeric compound of  claim 46 , wherein said linking moiety comprises a phosphodiester, phosphotriester, hydrogen phosphonate, alkylphosphonate, alkylphosphonothioate, arylphosphonothioate, phosphorothioate, phosphorodithioate, or phosphoramidate.  
     
     
         54 . The oligomeric compound of  claim 46  having a plurality of monomeric sub-units of said formula.  
     
     
         55 . The oligomeric compound of  claim 54  wherein said monomeric sub-units are located at preselected positions.

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