US2015183750A1PendingUtilityA1

5-fluoro-4-imino-3-(alkyl/substituted alkyl)-1-(arylsulfonyl)-3,4-dihydropyrimidin-2(1h)-one and processes for their preparation

Assignee: DOW AGROSCIENCES LLCPriority: Dec 31, 2013Filed: Dec 29, 2014Published: Jul 2, 2015
Est. expiryDec 31, 2033(~7.4 yrs left)· nominal 20-yr term from priority
A01N 43/54C07D 239/47C07D 333/10C07D 409/06C07D 239/24
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Claims

Abstract

Provided herein are 5-fluoro-4-imino-3-(alkyl/substituted alkyl)-1-(arylsulfonyl)-3,4-dihydropyrimidin-2(1H)-one and processes for their preparation which may include the use of an alkali alkoxide and an alkylating agent

Claims

exact text as granted — not AI-modified
What is claimed is: 
     
         1 . A method of making compounds of Formula III, including the steps of:
 contacting a compound of Formula II with an alkali alkoxide and an alkylating agent,   
       
         
           
           
               
               
           
         
       
       and forming a compound of Formula III: 
       
         
           
           
               
               
           
         
       
       wherein R 1  is selected from the group consisting of: 
       
         
           
           
               
               
           
         
       
       and R 2  is selected from the group consisting of: 
       
         
           
           
               
               
           
         
       
     
     
         2 . The method of  claim 1 , wherein the contacting step is carried out between 22° C. and 60° C. 
     
     
         3 . The method of  claim 1 , wherein the contacting step further includes a solvent selected from the group consisting of DMF, DMSO, DMA, NMP, and CH 3 CN. 
     
     
         4 . The method of  claim 1 , wherein the alkali alkoxide is selected from the group consisting of: KO t Bu, CH 3 ONa, CH 3 CH 2 ONa, CH 3 CH 2 OLi, CH 3 OLi, CH 3 CH 2 OK, and CH3CH 2 ONa. 
     
     
         5 . The method of  claim 1 , wherein the alkylating agent is selected from the group consisting of: alkyl halides and benzyl halides. 
     
     
         6 . The method of  claim 5 , wherein the alkyl halides and benzyl halides are selected from the group consisting of: methyl iodide, ethyl iodide, and benzyl bromide. 
     
     
         7 . The method of  claim 3 , wherein the alkali alkoxide is KO t Bu, and the solvent is DMF. 
     
     
         8 . The method of  claim 2 , wherein a molar ratio of the compound of Formula II to alkali alkoxide is from about 3:1 to about 1:1 and a molar ratio of the compound of Formula II to alkylating agent is from about 1:1 to about 3:1. 
     
     
         9 . The method of  claim 8 , wherein a molar ratio of the compound of Formula II to alkali alkoxide base is about 2:1 and a molar ratio of the compound of Formula II to alkylating agent is about 1:3. 
     
     
         10 . The method of  claim 9 , further including the step of diluting a completed reaction mixture with CH 3 CN and 2.5% aqueous Na 2 S 2 O 3 . 
     
     
         11 . The method of  claim 10 , wherein a ratio of DMF to CH 3 CN is from about 1:1 to about 3:1 and a ratio of DMF to 2.5% aqueous Na 2 S 2 O 3  is from about 1:2 to about 2:1. 
     
     
         12 . The method of  claim 11 , wherein a ratio of DMF to CH 3 CN is about 2:1 and a ratio of DMF to 2.5% aqueous Na 2 S 2 O 3  is about 1:1. 
     
     
         13 . A method of preparing a compound of Formula II, including the steps of:
 contacting a compound of Formula I:   
       
         
           
           
               
               
           
         
       
       with bis-N,O-trimethylsilylacetamide; and
 forming a compound of Formula II: 
 
       
         
           
           
               
               
           
         
       
       wherein R 1  is selected from the group consisting of: 
       
         
           
           
               
               
           
         
       
       and R 2  is selected from the group consisting of: 
       
         
           
           
               
               
           
         
         wherein a molar ratio of the compound of Formula Ito bis-N,O-trimethylsilylacetamide is 1:1.1 and the contacting step is carried out at about 22° C. to about 70° C. 
       
     
     
         14 . The method of  claim 13 , wherein the contacting step further includes contacting the compound of Formula I with CH 3 CN. 
     
     
         15 . The method of  claim 14 , further comprising the step of contacting a bis-N,O-trimethylsilylacetamide treated reaction mixture with an arylsulfonyl chloride. 
     
     
         16 . The method of  claim 15 , wherein a molar ratio of the compound of Formula Ito arylsulfonyl chloride is from about 1:2 to about 2:1. 
     
     
         17 . The method of  claim 16 , wherein a molar ratio of the compound of Formula Ito arylsulfonyl chloride is about 1:1.1.

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