Dimethyl 2,2-dimethyl-3-oxobutanedioate → HCID 178500128、化合物
反応式
[CH3:1][C:2]([CH3:13])([C:7](=O)[C:8](OC)=[O:9])[C:3]([O:5][CH3:6])=[O:4].[F:14][C:15]1[CH:34]=[CH:33][CH:32]=[CH:31][C:16]=1[CH2:17][N:18]1[C:22]2=[N:23][CH:24]=[N:25][CH:26]=[C:21]2[C:20]([C:27](=[NH:30])[NH:28][NH2:29])=[N:19]1>C(O)C>[F:14][C:15]1[CH:34]=[CH:33][CH:32]=[CH:31][C:16]=1[CH2:17][N:18]1[C:22]2=[N:23][CH:24]=[N:25][CH:26]=[C:21]2[C:20]([C:27]2[N:28]=[N:29][C:7]([C:2]([CH3:13])([CH3:1])[C:3]([O:5][CH3:6])=[O:4])=[C:8]([OH:9])[N:30]=2)=[N:19]1参加物
4
実験手順
584 mg (3.103 mmol) of dimethyl 2,2-dimethyl-3-oxobutanedioate were initially charged in 12 ml of ethanol and heated to reflux. Subsequently, 590 mg (2.069 mmol) of 1-(2-fluorobenzyl)-1H-pyrazolo[3,4-d]pyrimidine-3-carboximidohydrazide suspended in 12 ml of ethanol were added and the mixture was boiled under reflux overnight. After cooling, the mixture was filtered, the filtercake was washed with a little ethanol and the filtrate was concentrated. The residue was stirred with 10 ml of acetonitrile. 188 mg of the target compound were obtained (purity 93%; 20% of theory).