Triazole pyrimidine sulphonates compound, preparing method and application thereof
A technology of azolopyrimidine sulfonate and compound, applied in the field of triazolopyrimidine sulfonate compound and its preparation and application
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Embodiment 1
[0034] Example 1 Synthesis of O-(1,2,4-triazolo[1,5-a]pyrimidin-2-yl)-4-methylbenzenesulfonate (compound 1)
[0035] In a 50mL three-necked flask, add 0.66g (0.004mol) 2-hydroxyl-5,7-dimethyl-1,2,4-triazol[1,5-a]pyrimidine, 0.16g (0.004mol) hydroxide Sodium, 20mL water, dissolved by magnetic stirring, drop into 5mL ether solution of 0.77g (0.004mol) p-toluenesulfonyl chloride at room temperature, about 0.5h after dripping, there is solid formation, continue to stir for 5h, distill off the ether under reduced pressure, pump The gray solid was obtained by filtration, washed with 3% hydrochloric acid aqueous solution and 5% sodium bicarbonate aqueous solution respectively, and then washed several times with water, dried, and subjected to silica gel column chromatography, petroleum ether-acetone (50 / 50, v / v) as solvent , to obtain colorless flaky crystal compound 1 with a yield of 85.0% and a melting point of 149°C to 151°C.
[0036] 1 H NMR (internal standard TMS, solvent is CD...
Embodiment 20
[0040] Synthesis of Example 20-(1,2,4-triazolo[1,5-a]pyrimidin-2-yl)-benzenesulfonate (compound 2)
[0041] In a 50mL three-necked flask, add 0.66g (0.004mol) 2-hydroxyl-5,7-dimethyl-1,2,4-triazol[1,5-a]pyrimidine, 0.16g (0.004mol) hydroxide Sodium, 20mL water, magnetically stirred to dissolve, drop 0.71g (0.004mol) benzenesulfonyl chloride in 5mL ether solution at room temperature, after about 0.5h, a solid was formed, continue to stir for 5h, distill off the ether under reduced pressure, filter with suction A gray solid was obtained, which was washed with 3% hydrochloric acid aqueous solution and 5% sodium bicarbonate aqueous solution, and then washed several times with water, dried, and subjected to silica gel column chromatography, petroleum ether-acetone (70 / 30, v / v) as solvent, Compound 2 was obtained as colorless columnar crystals with a yield of 88.0% and a melting point of 145°C to 147°C.
[0042] 1 H NMR (internal standard TMS, solvent is CDCl 3 ): δppm
[0043] ...
Embodiment 30
[0046] Synthesis of Example 30-(1,2,4-triazolo[1,5-a]pyrimidin-2-yl)-4-nitrobenzenesulfonate (compound 3)
[0047] In a 50mL three-necked flask, add 0.66g (0.004mol) 2-hydroxy-5,7-dimethyl-1,2,4-triazol[1,5-a]pyrimidine, 0.21g (0.004mol) sodium carbonate , 20mL of water, magnetically stirred to dissolve, drop 0.89g (0.004mol) 4-nitrobenzenesulfonyl chloride in 10mL of methyl tert-butyl ether solution at room temperature, after about 0.5h, a solid was formed, continue to stir for 5h, Methyl tert-butyl ether was evaporated under reduced pressure, a gray solid was obtained by suction filtration, washed with 3% hydrochloric acid aqueous solution and 5% sodium bicarbonate aqueous solution, and then washed several times with water, dried, and subjected to silica gel column chromatography, petroleum ether- Acetone (70 / 30, v / v) was used as solvent to obtain white columnar crystal compound 3 with a yield of 92.0%.
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