1-substituted-1H-1,2,4-triazole-formamide derivatives, preparation and application thereof
A 1H-1, derivative technology, applied in the field of chemistry, can solve the problems of patient side effects, damage, ineffectiveness, etc.
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Embodiment 1
[0020] Example 1, methyl-1-(2,6-difluorobenzyl)-1 H -1,2,4-triazole-5-carboxylate (Ⅲ a ) and methyl-1-(2,6-difluorobenzyl)-1 H -1,2,4-triazole-3-carboxylate (Ⅳ a )
[0021] Methyl-1 H -1,2,4-Triazole-3-carboxylate (128 mg, 1.0 mmol) was dissolved in N,N-dimethylformamide (2.4 mL), and sodium hydride (48 mg) was added at room temperature, stirred for 10 minutes, 2,6-difluorobenzyl chloride (162 mg, 1.0 mmol) was added and reacted at 70 °C for about 2 hours. Add water (15 mL) to quench the reaction, extract with ethyl acetate (15 mL×3), and dry the organic layer over anhydrous sodium sulfate. : 1) Carry out column chromatography separation, can obtain
[0022] ①Pale yellow solid 16.7 mg, yield 6%; melting point: 86.3-87.5 °C.
[0023] 1 H NMR (500 MHz, CDCl 3 ): 7.96 (s, 1H), 7.36 (m, 1H), 6.96 (t, 2H, J = 7.5 Hz), 5.96 (s, 2H), 4.06 (s, 3H); 13 C-NMR (125 MHz, CDCl 3 ): 162.74, 160.69, 158.61, 151.32, 144.54, 131.25, 111.92, 111.76, 111.32, 53.45, 42.38.
[0024] ...
Embodiment 2
[0027] Embodiment 2, methyl-1-(2-chlorobenzyl)-1 H -1,2,4-triazole-5-carboxylate (Ⅲ b ) and methyl-1-(2-chlorobenzyl)-1 H -1,2,4-triazole-3-carboxylate (Ⅳ b )
[0028] The operating process is the same as in Example 1, except that 2,6-difluorobenzyl chloride is replaced with 2-chlorobenzyl chloride to obtain
[0029] ①Pale yellow crystals, yield: 6%; melting point: 86.8-87.8 °C.
[0030] 1 H NMR (500 MHz, CDCl 3 ): 8.06 (s, 1H), 7.43 (d, 1H, J = 8 Hz), 7.29 (t, 1H, J = 6 Hz), 7.23 (t, 1H, J = 7.5 Hz), 6.87 (d, 1H, J= 6.5 Hz), 5.96 (s, 2H), 4.00 (s, 3H).
[0031] ②White solid, yield: 58%; melting point: 90.4-91.1 °C.
[0032] 1 H NMR (500 MHz, CDCl 3 ): 8.19 (s, 1H), 7.46 (d, 1H, J = 8 Hz), 7.36 (m, 1H), 7.32 (m, 2H), 5.55 (s, 2H), 4.00 (s, 3H).
[0033]
Embodiment 3
[0034] Example 3, methyl-1-((2-chloropyridine-3-substituted) methyl)-1 H -1,2,4-triazole-5-carboxylate (Ⅲ c ) and methyl-1-((2-chloropyridine-3-substituted) methyl)-1 H -1,2,4-triazole-3-carboxylate (Ⅳ c )
[0035] The operation process is the same as in Example 1, except that 2,6-difluorobenzyl chloride is replaced with 3-(bromomethyl)-2-chloropyridine to obtain
[0036] ①Pale yellow solid, yield: 22%; melting point: 87.0-88.1 °C.
[0037] 1 H NMR (500 MHz, CDCl 3 ): 8.39 (d, 1H, J = 7.5 Hz), 8.10 (s, 1H), 7.24 (m, 1H), 7.19 (m, 1H), 5.96 (s, 2H), 4.02 (s, 3H).
[0038] ②White solid, yield: 51%; melting point: 90.7-91.5 °C.
[0039] 1 H NMR (500 MHz, CDCl 3 ): 8.44 (d, 1H, J = 4.5 Hz), 8.34 (s, 1H), 7.63 (d, 1H, J = 8 Hz), 7.33 (t, 1H, J = 4.5 Hz), 5.57 (s, 2H), 4.02 (s, 3H).
[0040]
PUM
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