Cl[C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([N+:8]([O-:10])=[O:9])[C:3]=1[S:11]([NH2:14])(=[O:13])=[O:12].CS(C)=O.[CH2:19]([NH:21][CH2:22]C)C.[F-].[K+]>[N+](CCCC)(CCCC)(CCCC)CCCC.[O-]S(O)(=O)=O.O>[CH3:19][N:21]([CH3:22])[C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([N+:8]([O-:10])=[O:9])[C:3]=1[S:11]([NH2:14])(=[O:13])=[O:12]A mixture of 2-chloro-6-nitro-benzenesulfonamide (500 mg, 2.10 mmol), DMSO (3 ml), diethyl amine (10 ml of 2 M solution in THF), Bu4NHSO4 (34 mg, 0.1 mmol) and KF (58 mg, 1.0 mmol) is heated in an autoclave at 70° C. for 16 h. The mixture is diluted with water and extracted with CH2Cl2. The solvent is removed and the residue subjected to chromatography (SiO2, TBME/cyclohexane 1:9→TBME) to give 2-dimethylamino-6-nitro-benzenesulfonamide as a colorless solid.
Wird geladen…
