Preparation and bactericidal activity of N-pyridyl-substituted thiazole methanamide compounds
A technology based on thiazole carboxamide and pyridyl, which is applied in the fields of fungicides, organic chemistry, biocides, etc.
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Embodiment 1
[0012] Add 0.01mol of 2-methyl-4-trifluoromethylthiazole carboxylic acid chloride, 30ml of toluene, 0.01mol of 3-chloro-5-trifluoromethyl-2-aminopyridine, 0.01g of triethylamine into the three-necked flask, Heat to reflux, react for 8 hours, evaporate to remove the solvent, add 20ml of water and stir for 30min, the aqueous phase is extracted with ethyl acetate, and the organic phase is extracted with 10% NaHCO 3 , water, brine, and spin-dried to obtain a crude product. The resulting solid was separated by recrystallization to obtain the target compound a with a yield of 73.5%. Compound a is a white solid powder. Melting point: 128-129°C. MS: 390.2 (m / z, M+1). 1 H NMR (500MHz, CDCl 3 ): 2.786 (s, 3H, CH 3 ), 8.005-8.009 (d, 1H, Py-H), 8.592 (s.1H, Py-H), 8.613 (s, 1H, NH).
Embodiment 2
[0014] Add 0.01mol of 2-methyl-4-trifluoromethylthiazoleformyl chloride, 30ml of toluene, 0.01mol of 3-chloro-2-aminopyridine, 0.01g of triethylamine into the three-neck flask, heat to reflux, and react for 8 hours , evaporated to remove the solvent, added 20ml of water and stirred for 30min, the aqueous phase was extracted with ethyl acetate, and the organic phase was extracted with 10% NaHCO 3 , water, brine, and spin-dried to obtain a crude product. The resulting solid was separated by recrystallization to obtain the target compound c with a yield of 68.4%. Compound c is a white solid powder. Melting point: 133-134°C. MS: 322.1 (m / z, M+1). 1 H NMR (500MHz, CDCl 3 ): 2.770 (s, 3H, CH 3 ), 7.128-7.154 (m, 1H, Py-H), 7.786-7.806 (m, 1H, Py-H), 8.327-8.335 (m, 1H, Py-H), 9.499 (s, 1H, NH).
Embodiment 3
[0016] Add 0.01mol of 2-methyl-4-trifluoromethylthiazoleformyl chloride, 30ml of toluene, 0.01mol of 4-chloro-2-aminopyridine, 0.01g of triethylamine into the three-neck flask, heat to reflux, and react for 8 hours , evaporated to remove the solvent, added 20ml of water and stirred for 30min, the aqueous phase was extracted with ethyl acetate, and the organic phase was extracted with 10% NaHCO 3 , washed with water, brine, and spin-dried to obtain a crude product, and the resulting solid was separated by column chromatography to obtain the target compound d with a yield of 72.5%. Compound d is a gray solid powder. Melting point: 186-187°C. MS: 322.2 (m / z, M+1). 1 H NMR (500MHz, CDCl 3 ): 2.758 (s, 3H, CH 3 ), 7.064-7.089 (m, 1H, Py-H), 7.753-7.787 (m, 1H, Py-H), 8.048-8.058 (d, 1H, Py-H), 8.247-8.264 (d, 1H, Py-H -H), 9.487 (s, 1H, NH).
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