Preparation method of 3, 3'-di(trifluouro methyl) phenyl methane
A technology of trifluoromethylbenzene and trifluoromethyl, applied in the field of preparation of organic fluorine compounds, can solve the problems of high production cost, easy volatility, and difficulty in realizing industrialized production, and achieves low production cost, low environmental pollution, and low operation cost. handy effect
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Embodiment 1
[0010] Example 1 3,3'-two (trifluoromethyl) benzene methane preparation
[0011] Add 60g80%H in a 500ml three-neck flask 2 SO 4 solution, then add 200g (1.08mol) trifluoromethylbenzene, 13g (0.43mol) 98% paraformaldehyde (melting point 121-123°C), place it in an ice-water bath at 0°C, add dropwise 63g (0.54mol) chlorosulfur Acid, dropwise at a temperature of 10-25°C, stir for 15 minutes, react at 30°C for 6 hours, and remove the acidic water phase in the lower layer. The upper organic phase was washed twice with 500ml of water, then neutralized to pH 5-6 with 5% NaOH solution, and the organic phase was measured by gas chromatography, wherein the content of 3,3'-bis(trifluoromethyl)benzenemethane was 62.4%. .
[0012] Put the above-mentioned organic phase in a 500ml three-neck flask, heat and distill under reduced pressure, distill off 80g of the front fraction at a vacuum of 0.098Mpa and a temperature of 50-80°C, and remove unreacted trifluoromethylbenzene (which can be use...
Embodiment 2
[0022] Embodiment 2 3, the preparation of 3'-two (trifluoromethyl) benzene methane
[0023] Add 70g of 70% H in a 500ml three-neck flask 2 SO 4 solution, then add 200g (1.08mol) trifluoromethylbenzene, 29g (0.97mol) 98% paraformaldehyde (melting point 121-123°C), place it in an ice-water bath at 0°C, and add 126g (1.08mol) chlorosulfur dropwise Acid, dropwise temperature 5-15°C, then react at 40°C for 3 hours, separate the lower acidic aqueous phase, and use gas chromatography to determine the organic phase, where C 15 h 10 f 6 The content is 50.2%.
[0024] Put the above organic phase in a 500ml three-necked flask, heat and distill under reduced pressure, distill off the front fraction (98g) at a vacuum of 0.098Mpa and a temperature of 50-80°C to obtain 102g of distillation raffinate, put it in -5°C freezing liquid for 3 hours Finally, the material is in a molten state, quickly put it into the funnel for suction filtration, wash the filter cake with water, and drain it f...
Embodiment 3
[0025] Embodiment 3 3, the preparation of 3'-two (trifluoromethyl) benzene methane
[0026] Add 90g of 90% H in a 500ml three-necked flask 2 SO 4 solution, then add 200g (1.08mol) trifluoromethylbenzene, 16g (0.54mol) 98% paraformaldehyde (melting point 121-123°C), place it in an ice-water bath at 0°C, add dropwise 88g (0.76mol) chlorosulfur Acid, dropwise temperature 10-25°C, then react at 40°C for 4 hours, separate the lower layer of acid water phase, and use gas chromatography to determine the organic phase, where C 15 h 10 f 6 The content is 72.4%.
[0027] Put the above-mentioned organic phase in a 500ml three-neck flask, heat and distill under reduced pressure, and distill it out at a vacuum of 0.098Mpa and a temperature of 50-80°C. After one hour, the material is in a molten state, put it into the funnel for suction filtration quickly, wash the filter cake with water, and drain it for later use. The filtrate was repeatedly frozen once, and suction filtered to obta...
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