[Cl:1][C:2]1[N:7]=[N:6][C:5](/[N:8]=[C:9](\Cl)/[C:10]([F:13])([F:12])[F:11])=[CH:4][CH:3]=1.C[O:16][NH2:17]>O1CCCC1>[Cl:1][C:2]1[N:7]=[N:6][C:5]([NH:8]/[C:9](=[N:17]\[OH:16])/[C:10]([F:13])([F:12])[F:11])=[CH:4][CH:3]=1To a solution of 4.5 g (18 mmol) of the crude product of Step B in 150 mL tetrahydrofuran was carefully added 2 mL aqueous 50% methoxyamine. The resulting solution was stirred under nitrogen at ambient temperature. After 1 h the solution was concentrated in vacuo then dissolved in 100 mL ethyl acetate and washed sequentially with saturated aqueous sodium bicarbonate solution and saturated aqueous brine (100 mL each). The organic phase was then dried over magnesium sulfate, filtered, and evaporated in vacuo to yield a crude oil.
Wird geladen…