Sodium Bicarbonate → 4-[2,5-Dioxo-4-(4-fluorophenyl)-4-hydroxymethyl-3-methylimidazolidin-1-yl]-2-trifluoromethylbenzonitrile
反応式
[O:1]=[C:2]1[N:6]([CH3:7])[C:5]([C:13]2[CH:18]=[CH:17][C:16]([F:19])=[CH:15][CH:14]=2)([CH2:8][O:9]CC=C)[C:4](=[O:20])[N:3]1[C:21]1[CH:28]=[CH:27][C:24]([C:25]#[N:26])=[C:23]([C:29]([F:32])([F:31])[F:30])[CH:22]=1.C(=O)(O)[O-].[Na+]>C(Cl)Cl>[O:1]=[C:2]1[N:6]([CH3:7])[C:5]([C:13]2[CH:14]=[CH:15][C:16]([F:19])=[CH:17][CH:18]=2)([CH2:8][OH:9])[C:4](=[O:20])[N:3]1[C:21]1[CH:28]=[CH:27][C:24]([C:25]#[N:26])=[C:23]([C:29]([F:31])([F:32])[F:30])[CH:22]=1参加物
4
反応物 2
生成物 1
試薬・触媒・溶媒 1
実験手順
The crude mixture of 4-[2,5-dioxo-4-(4-fluorophenyl)-3-methyl-4-[(2-propenyloxy)methyl]imidazolidin-1-yl]-2-trifluoromethylbenzonitrile obtained in step 5 is solubilised in 5 mL of DCM under argon atmosphere. 0.9 mL of trifluoroborane-dimethylsulfide complex is added. The mixture is stirred at rt for 7 hours. A saturated aqueous sodium bicarbonate solution is added slowly, the product is extracted with DCM and the organic layer is dried over sodium sulfate, filtered and evaporated. The crude product is purified by chromatography over silica gel while eluting with 4/1 DCM/ethyl acetate.