Patent ID: 8183390
Filing Date: 2012-05-22
Classification: C07D,C08F,C08G

Abstract:
1. A process for preparing thiophene substituted 1,3-Dithien-2-yl-2,2-disubstituted propane-1,3-dione (DMDTPy) comprising: wherein R1 is selected from the group consisting of: hydrogen; alkyl from 1 to about 22 carbon atoms; alkoxy from 1 to about 22 carbon atoms; nitro; halogen; cyano ester; mono- & di-alkylamine from 1 to about 22 carbon atoms; ester groups from 1 to about 22 carbon atoms; amide from 1 to 22 carbon atoms; alcohol from 1 to 22 carbon atoms; amino; sulphonate groups; silyl; perfluoro alky from 1 to about 22 carbon atoms; wherein R2 is selected from the group consisting of: hydrogen; alkyl from 1 to about 22 carbon atoms; alkoxy from 1 to about 22 carbon atoms; nitro; halogen; cyano ester; mono- & di-alkylamine from 1 to about 22 carbon atoms; ester groups from 1 to about 22 carbon atoms; amide from 1 to 22 carbon atoms; alcohol from 1 to 22 carbon atoms; amino; sulphonate groups; silyl; perfluoro alky from 1 to about 22 carbon atoms; wherein R3 is selected from the group consisting of: hydrogen; alkyl from 1 to about 22 carbon atoms; alkoxy from 1 to about 22 carbon atoms; nitro; halogen; cyano ester; mono- & di-alkylamine from 1 to about 22 carbon atoms; ester groups from 1 to about 22 carbon atoms; amide from 1 to 22 carbon atoms; alcohol from 1 to 22 carbon atoms; amino; sulphonate groups; silyl; perfluoro alky including from 1 to about 22 carbon atoms; dissolving 3-substituted 2-bromothiophene in dry diethyl ether to form a first composition; dissolving n-butyl lithium in hexanes to form a second composition; combining said first composition and said second composition to form a third composition; stirring said third composition for a predetermined time, allowing contact of reactants, to form a fourth composition; dissolving ZnCl adding said fifth composition to said fourth composition to form a sixth composition; warming said sixth composition to room temperature to form a seventh composition; refluxing said seventh composition for a predetermined time, allowing further contact of reactants, to form an eighth composition; cooling said eighth composition to room temperature to form a ninth composition; adding tetrakis-(triphenylphosphine)palladium (0) to said ninth composition to form a tenth composition; adding disubstituted malonyl chloride to said tenth composition to form an eleventh composition; refluxing said eleventh composition for a predetermined time with stirring, allowing further contact of reactants, to form an twelfth composition; mixing said twelfth composition with saturated aqueous sodium bicarbonate to form a two-phase mixture having an aqueous phase and a first organic phase; separating said first organic phase from said aqueous phase; washing said first organic phase with brine to form a two-phase mixture having a brine phase and a second organic phase; separating said second organic phase from said brine phase; drying said second organic phase; removing the solvent from said second organic phase to form a residue containing thiophene substituted 1,3-Dithien-2-yl-2,2-disubstituted propane-1,3-dione (DMDTPy); and extracting DMDTPy from said residue.