Piperazine → HCID 14459477、化合物
反応式
[F:1][C:2]1[CH:3]=[C:4]([C:9]2[CH:10]([CH3:16])[CH2:11][C:12](=[O:15])[NH:13][N:14]=2)[CH:5]=[CH:6][C:7]=1F.[NH:17]1[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1>ClCCl>[F:1][C:2]1[CH:3]=[C:4]([C:9]2[CH:10]([CH3:16])[CH2:11][C:12](=[O:15])[NH:13][N:14]=2)[CH:5]=[CH:6][C:7]=1[N:17]1[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1参加物
4
実験手順
5.0 g (22.3 mmol) of 6-(3,4-difluorophenyl)-4,5-dihydro-5-methyl-3(2H)-pyridazinone and 19.2 g (222 mmol) of piperazine are stirred at 160° C. for 15 hours. When the reaction mixture has cooled down, it is taken up with 200 ml of dichloromethane and washed with 3×30 ml of water. After drying, the organic phase is concentrated by evaporation and the residue is crystallized with methanol. The solid obtained is suction filtered and recrystallized from ethyl acetate. 3.5 g (54%) of colourless crystals, m.p. 172°-174° C., are obtained.