[Cl:1][C:2]1[CH:9]=[C:8]([S:10]([CH3:13])(=[O:12])=[O:11])[CH:7]=[CH:6][C:3]=1[C:4]#[N:5].[NH2:14][OH:15]>C(O)C>[Cl:1][C:2]1[CH:9]=[C:8]([S:10]([CH3:13])(=[O:12])=[O:11])[CH:7]=[CH:6][C:3]=1[C:4](=[N:14][OH:15])[NH2:5]The nitrile from Step B was dissolved into 100 mL of 1:1 ethanol/50% aqueous hydroxylamine then heated to reflux for 12 h. After evaporation of the solvent, the residue was dissolved into 400 mL of ethyl acetate then washed with saturated aqueous brine (150 mL). The organic phase was dried over magnesium sulfate, filtered, and evaporated in vacuo to yield the title compound, which was used without further purification. LC/MS 449.05 (M+1), 451.03 (M+3).
Wird geladen…