[F:1][C:2]1[N:7]=[C:6]([F:8])[CH:5]=[C:4]([F:9])[N:3]=1.C(=O)([O-])[O-].[K+].[K+].[C:16]([N:19]1[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]1)(=[O:18])[CH3:17].O>C(#N)C>[C:16]([N:19]1[CH2:24][CH2:23][N:22]([C:2]2[N:7]=[C:6]([F:8])[CH:5]=[C:4]([F:9])[N:3]=2)[CH2:21][CH2:20]1)(=[O:18])[CH3:17].[C:16]([N:19]1[CH2:24][CH2:23][N:22]([C:6]2[CH:5]=[C:4]([F:9])[N:3]=[C:2]([F:1])[N:7]=2)[CH2:21][CH2:20]1)(=[O:18])[CH3:17]To a solution of 2,4,6-trifluoropyrimidine (2.0 g) and potassium carbonate (3.1 g) in acetonitrile (15 ml) was added a solution of 1-acetylpiperazine (1.9 g) in acetonitrile (5 ml) over 10 min under ice-cooling and the mixture was stirred at room temperature for 1 hr. The reaction mixture was poured into water and extracted with ethyl acetate. The extract was washed with brine and dried over anhydrous sodium sulfate. The solvent was evaporated to give a pale-yellow oil. The obtained pale-yellow oil was purified by silica gel column chromatography to give the title compound (1.8 g) and 1-acetyl-4-(2,6-difluoropyrimidin-4-yl)piperazine (1.7 g) both as a white solid.
Loading…