Dimethyl 2,2-dimethyl-3-oxobutanedioate → HCID 178500133、化合物
反応式
[F:1][C:2]1[CH:3]=[C:4]2[C:10]([C:11](=[NH:14])[NH:12][NH2:13])=[N:9][N:8]([CH2:15][C:16]3[C:21]([F:22])=[CH:20][CH:19]=[C:18]([F:23])[C:17]=3[F:24])[C:5]2=[N:6][CH:7]=1.[CH3:25][C:26]([CH3:37])([C:31](=O)[C:32](OC)=[O:33])[C:27]([O:29][CH3:30])=[O:28]>C(O)C>[F:1][C:2]1[CH:3]=[C:4]2[C:10]([C:11]3[N:12]=[N:13][C:31]([C:26]([CH3:37])([CH3:25])[C:27]([O:29][CH3:30])=[O:28])=[C:32]([OH:33])[N:14]=3)=[N:9][N:8]([CH2:15][C:16]3[C:21]([F:22])=[CH:20][CH:19]=[C:18]([F:23])[C:17]=3[F:24])[C:5]2=[N:6][CH:7]=1参加物
4
反応条件
- 温度
- 50 °C
実験手順
6.85 g (20.271 mmol) of the compound from Example 81A were dissolved in 300 ml of ethanol, 7.629 g (40.542 mmol) of dimethyl 2,2-dimethyl-3-oxobutanedioate (described in J. Am. Chem. Soc. 124(14), 3680-3691; 2002) were added and the mixture was stirred at 50° C. overnight. After cooling, a precipitate was filtered off and washed with ethanol. The filtrate was concentrated and then purified by preparative HPLC (methanol:water-75:25). This gave 3.30 g (33% of theory) of the title compound.