Methylamine → HCID 11024311、化合物

反応式

Br[C:2]1[CH:7]=[C:6]([S:8]([C:11]2[CH:16]=[CH:15][C:14]([NH2:17])=[CH:13][CH:12]=2)(=[O:10])=[O:9])[CH:5]=[C:4]([Br:18])[N:3]=1.[CH3:19][NH2:20]>O1CCOCC1.C(O)C>[NH2:17][C:14]1[CH:15]=[CH:16][C:11]([S:8]([C:6]2[CH:5]=[C:4]([Br:18])[N:3]=[C:2]([NH:20][CH3:19])[CH:7]=2)(=[O:10])=[O:9])=[CH:12][CH:13]=1

参加物

実験手順

1.45 g (0.0037 mol) of 4-(2,6-dibromopyridine-4-sulphonyl)-phenylamine were dissolved in 40 ml of dioxane and treated with 9.6 ml of 8M methylamine in ethanol. The mixture was stirred at room temperature for 48 hrs., the solvents were removed and the residue was chromatographed on silica gel with ethyl acetate/hexane 1:3 and 1:2. The product-containing fractions, after concentration, were suspended in 50 ml of diethyl ether, treated in an ultrasound bath for 1 hr., then treated with 75 ml of hexane and the precipitate which thereby resulted was filtered off under suction. After drying in a high vacuum there was obtained 0.87 g (69%) of [4-(4-aminobenzenesulphonyl)-6-bromopyridin-2-yl]-methylamine as pale beige crystals; m.p.: 171-173° C.