Dimethylformamide → HCID 54373171、化合物
反応式
[H-].[Na+].[N:3]1[CH:8]=[CH:7][N:6]=[CH:5][C:4]=1C1C=CC(=O)NC=1.[CH3:16][C:17]1C=CC(S(C)(=O)=O)=C[CH:22]=1.[CH3:27][N:28]([CH:30]=[O:31])[CH3:29]>>[CH3:27][N:28]1[CH:29]=[C:22]([N:3]2[CH:4]=[CH:5][N:6]=[CH:7][CH2:8]2)[CH:17]=[CH:16][C:30]1=[O:31]参加物
5
実験手順
Sodium hydride (0.75 g) is added to a stirred solution of 5-(2-pyrazinyl)-2(1H) pyridone (2.2 g) in DMF (150 ml). Methyl p-toluene sulfonate (4.0 g) is added to the stirred reaction mixture after 5 minutes of stirring. After 35 minutes reaction time at RT, the reaction mixture is filtered and the filtrate evaporated in vacuum. The oily solid residue is washed with ether, filtered and the dry solid treated with hot acetone. The acetone is filtered and the filtrate evaporated, yielding a solid. The ether filtrate from above is evaporated, yielding a solid which after washing with decane is combined with the acetone filtrate solid. The combined solids are recrystallized from toluene and decane (treated with charcoal and filtered while hot) resulting in the desired 1-methyl pyridone compound, M.P. 165.5°-166.5° C.