Benzyl chloride tertiary amine double azole antimicrobial compounds, preparation and medical use thereof
A technology of halogen benzyl tertiary amine dichloride compound and halogen benzyl tertiary amine, which is applied in the fields of organic chemistry and medicinal chemistry, and achieves the effects of low cost, simple and convenient synthesis method and readily available raw materials
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Embodiment 1
[0033] Example 1: N-(2-(1H-1,2,4-triazol-1-yl)ethyl)-N-(2,4-difluorobenzyl)-2-(1H-1,2 , the preparation of 4-triazol-1-yl) ethylamine (compound 1 for short)
[0034]Add 30mL of acetonitrile, 5.11g (37.0mmol) of anhydrous potassium carbonate and 2.24g (32.4mmol) of 1,2,4-triazole into a 100mL single-necked round bottom flask equipped with a condensing reflux tube and a drying tube, and stir to raise the temperature To 50°C, react for one hour, after cooling to room temperature, add 2-bromo-N-(2-bromoethyl)-N-(2,4-difluorobenzyl)ethylamine 5.52g (15.4mmol) under stirring . After the reaction was complete, the solvent was distilled off under reduced pressure, the residue was added with 20 mL of water, extracted three times with dichloromethane, all the dichloromethane layers were washed once with saturated brine, and then dried over anhydrous sodium sulfate. After the solvent was evaporated by rotary evaporation, 4.30 g of light yellow solid was obtained by column chromatograph...
Embodiment 2
[0035] Example 2: N-(2-(1H-imidazol-1-yl)ethyl)-N-(2,4-difluorobenzyl)-2-(1H-imidazol-1-yl)ethylamine (referred to as Compound 2) Preparation
[0036] Add 30mL of freshly distilled tetrahydrofuran, 1.04g (43.5mmol) of sodium hydride, and 2.53g (37.2mmol) of imidazole into the device. 2 In a 100mL three-necked round-bottomed flask with a protective device, stir and heat up to 50°C, react for one hour, and after cooling to room temperature, add 2-bromo-N-(2-bromoethyl)-N-(2,4- Difluorobenzyl)ethylamine 5.67g (15.9mmol). After the reaction was completed, the solvent was distilled off under reduced pressure, and the residue was added to the ice-water mixture under ice-water cooling, extracted three times with dichloromethane, all the dichloromethane layers were washed once with saturated brine, and then dried over anhydrous sodium sulfate. After rotary evaporation of the solvent, 4.52 g of a colorless liquid was obtained by column chromatography, that is, compound 2, and the yie...
Embodiment 3
[0037] Example 3: N-(2-(1H-1,2,4-triazol-1-yl)ethyl)-N-(2,4-dichlorobenzyl)-2-(1H-1,2 , the preparation of 4-triazol-1-yl) ethylamine (compound 3 for short)
[0038] According to the synthetic method of embodiment 1. 1,2,4-triazole 2.50g (36.0mmol), 2-bromo-N-(2-bromoethyl)-N-(2,4-dichlorobenzyl)ethylamine 5.86g (15.0mmol), Synthesis obtained 4.52 g of colorless viscous liquid, namely compound 3, with a yield of 82.3%. 1 H NMR (300MHz, CDCl 3 )δ: 8.10 (m, 4H, triazole 3-H, 5-H), 6.69~7.10 (m, 3H, Ar-H), 3.84 (bs, 4H, triazole 1 NCH 2 CH 2 ), 3.61 (s, 2H, PhCH 2 N), 2.80(t, 4H, triazole 1 NCH 2 CH 2 )ppm; MS (ESI, m / z): 366[M] + .
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