Preparation method of 2H-perfluoro (2-methylpentane)
A technology of methyl pentane and methyl, applied in the field of preparation of 2H-perfluoro, can solve the problems of harsh reaction conditions, large environmental pollution, low reaction yield and the like, and achieves the effects of mild conditions and low operating costs
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Embodiment 1
[0021] A 1000 ml four-necked flask is connected with a condensing reflux tube, and 100 grams of perfluoro-2-methyl-2-pentene is added in the 1000 ml four-necked flask, then 500 grams of acetonitrile and 1 gram of trimethylamine are added in acetonitrile solution (trimethylamine mass concentration 10%), cool down to 0°C, and pass through ozone at a flow rate of 500 mL / min (the concentration of ozone is 80g / m 3 ), kept for 5 hours, and stopped feeding ozone. The temperature was raised to 20°C, stirred for 2 hours, and finally directly rectified, and the fraction at 66-70°C was collected to obtain 53 grams of 2H-perfluoro(2-methylpentane) product, with a mass yield of 53%. According to gas chromatography analysis, the purity content of 2H-perfluoro (2-methylpentane) product is 99.5%.
[0022] MS (300.95, 129.5, 168.95, 168.95, 113.0, 69.05);
[0023] 1 H-NMR (CDCl 3 ):δ (ppm) 4.0(s, 1H);
[0024] 19 F-NMR (CDCl 3 ): δ (ppm) –62.061, -80.461, -111.987, -125.543.
[0025] T...
Embodiment 2
[0027] A condensing reflux tube is connected to a 1500 ml four-necked flask, and 100 grams of perfluoro-2-methyl-2-pentene is added to the 1500 ml four-necked flask, followed by 1000 grams of hydrofluoroether HFE-347 and 1 gram of triethylamine, cooled to 20°C, and passed into ozone at a flow rate of 500mL / min (the concentration of ozone is 100g / m 3 ), keep it for 2 hours, and stop feeding ozone. The temperature was raised to 50°C, stirred for 8 hours, and finally directly rectified, and the fraction at 66-70°C was collected to obtain 65 grams of 2H-perfluoro(2-methylpentane), with a mass yield of 65%. According to gas chromatography analysis, the purity content of 2H-perfluoro (2-methylpentane) product is 99.0%.
Embodiment 3
[0029] A condensing reflux tube is connected to a 1000 ml four-necked flask, and 100 grams of perfluoro-2-methyl-2-pentene is added to the 1000 ml four-necked flask, followed by 800 grams of hydrofluoroether HFE-347 and 0.8 gram of triethylamine, cooled to 10°C, and passed into ozone at a flow rate of 500mL / min (the concentration of ozone is 100g / m 3 ), keep it for 3 hours, and stop feeding ozone. The temperature was raised to 30°C, stirred for 5 hours, and finally directly rectified, and the fraction at 66-70°C was collected to obtain 68 grams of 2H-perfluoro(2-methylpentane), with a mass yield of 68%. Gas chromatography analysis shows that the purity content of 2H-perfluoro (2-methylpentane) product is 99.1%.
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