2.21 g |
With sodium hydroxide; In N,N-dimethyl-formamide; at 20℃; for 5h; |
0.60g (0.015 mol) of sodium hydroxide was added to a solution of 1.22g(0.0075 mol) of 2,5-dichloropyridin-3-amine in 40 mL of DMF, followed by addition of 2g (0.0075 mol) of <strong>[1897-41-2]2,3,5,6-<strong>[1897-41-2]tetrachloroterephthalonitrile</strong></strong> under stirring,the mixture was stirred for 5 h after addition at room temperature. After the reaction was over by Thin-Layer Chromatographymonitoring, the reaction mixture was poured into water and extracted with ethyl acetate, the organic phasewas washed with water and saturated brine, dried over anhydrous magnesium sulfate, filtered and then concentratedunder reduced pressure. The residue was purified through silica column (ethyl acetate/petroleum ether (boiling pointrange 60-90°C) = 1:3, as an eluent) to give 2.21 g of compound C-118 as yellow solid, m.p. 202-204°C.[0129] 1H-NMR (300MHz, internal standard TMS, solvent CDCl3) delta(ppm): 7.36(d, J=2.4Hz, 1H, Py-4-1H), 7.97(d,J=2.4Hz, 1H, Py-5-1 H), 8.89(br, 1H, NH). |
2.21 g |
With sodium hydroxide; In N,N-dimethyl-formamide; at 20℃; for 5h; |
0.60 g (0.015 mol) of sodium hydroxide was added to a solution of 1.22 g (0.0075 mol) of 2,5-dichloropyridin-3-amine in 40 mL of DMF, followed by addition of 2 g (0.0075 mol) of <strong>[1897-41-2]2,3,5,6-<strong>[1897-41-2]tetrachloroterephthalonitrile</strong></strong> under stirring, the mixture was stirred for 5 h after addition at room temperature. After the reaction was over by Thin-Layer Chromatography monitoring, the reaction mixture was poured into water and extracted with ethyl acetate, the organic phase was washed with water and saturated brine, dried over anhydrous magnesium sulfate, filtered and then concentrated under reduced pressure. The residue was purified through silica column (ethyl acetate/petroleum ether (boiling point range 60-90° C.)=1:3, as an eluent) to give 2.21 g of compound C-118 as yellow solid, m.p. 202-204° C. [0194] 1H-NMR (300 MHz, internal standard TMS, solvent CDCl3) delta (ppm): 7.36 (d, J=2.4 Hz, 1H, Py-4-1H), 7.97 (d, J=2.4 Hz, 1H, Py-5-1H), 8.89 (br, 1H, NH). |