Hydrochloric Acid → HCID 178447855, compound

Participants

Reaction Conditions

Reaction Steps

3.0 g (0.006 mol) of 2-(4'-bromo-3',5'-difluorophenyl)-5-[4'-(trans-4"-propylcyclohexyl)phenyl]pyrimidine and 0.8 g (0.08 mol) of copper (I) cyanide were added to 30 cm3 of NMP and the solution was refluxed for 2 hours using a mantle heater. The solution was cooled to 60° C. and added to a solution of 3.2 g of FeC13.6H2O, 1.0 cm3 of concentrated hydrochloric acid and 4 cm3 of water. The resulting solution was allowed to sit on a warm water bath at 60° C. for one hour. The crystals formed were filtered out, washed with water and treated through a silica gel column using chloroform as the solvent. The chloroform was distilled off and the residue was recrystallized from a solvent mixture of acetone and chloroform to yield 1.3 g (0.003 mol) of 2-(4'-cyano-3',5'-difluorophenyl)-5-[4 '-(trans-4"-propylcyclohexyl)phenyl]pyrimidine. The phase transition temperature of this compound, as measured by DSC, was: ##STR36##

Provenance & Evidence