[C:1]([NH:4][C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([N:11]2[CH:15]=[CH:14][N:13]=[CH:12]2)[CH:6]=1)(=[O:3])[CH3:2].[H-].[Na+].[H][H].F[C:21]1[CH:26]=[CH:25][C:24]([I:27])=[CH:23][C:22]=1[N+:28]([O-:30])=[O:29]>CN(C=O)C.O>[C:1]([N:4]([C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([N:11]2[CH:15]=[CH:14][N:13]=[CH:12]2)[CH:6]=1)[C:21]1[CH:26]=[CH:25][C:24]([I:27])=[CH:23][C:22]=1[N+:28]([O-:30])=[O:29])(=[O:3])[CH3:2]A solution of 2e from Example 3 (30 g, 0.15 mol) in dry DMF (200 ml) is cooled to 0° C. under nitrogen. Sodium hydride (7.2 g of a 60% dispersion in mineral oil) is added portionwise. When the evolution of hydrogen has ceased a solution of 1c from Example 1 (52 g, 0.19 mol) in 50 ml DMF is added. The mixture is stirred at 120° C. for 5 hours and left at ambient temperature over night. The reaction mixture is poured into four volumes of water and the crude product is filtered off. Purification on silica gel using a mixture of ethyl acetate and petroleum ether (3:17) as the eluent affords pure 6c as an oil (17 g, 25%).
불러오는 중…
