Method for preparing 1,4-bis(dichloromethyl) tetrafluorobenzene
A technology of dichloromethyl and tetrafluorobenzene is applied in the field of preparation of 1,4-bis(dichloromethyl)tetrafluorobenzene, and can solve the problems of long reaction time, low yield, unsuitability for mass production and the like
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Embodiment 1
[0050] Example 1: Preparation of 1,4-bis(dichloromethyl)tetrafluorobenzene (with toluene as solvent and dimethylformamide as catalyst)
[0051] Add 15.45gm of tetrafluoroterephthalaldehyde (TFTPA), 3.01gm of dimethylformamide (DMF) and 15.01gm of toluene into a 250ml three-port glass reactor (with temperature probe, condenser tube and ventilation tube) , under nitrogen, slowly add 63.37gm of SOCl from the temperature probe port to the feeding funnel 2 . Then, after replacing the feeding funnel with a temperature probe, start heating with an oil bath and stir with a magnetic stirrer. At this time, the nitrogen can be turned off, and the reflux reaction (85 to 95° C.) is performed for two hours, and gas chromatography (Gas Chromatography; GC) showed that the reaction was complete. After the reaction solution was cooled to room temperature, slowly introduce ice water to remove excess SOCl 2 Hydrolyzed, the water layer was separated after standing for stratification. Then, an ...
Embodiment 2 16
[0057] Embodiment two to sixteen: preparation 1,4-bis(dichloromethyl)tetrafluorobenzene
[0058] The preparation method of embodiment two to sixteen is the same as embodiment one. The amounts of related reactants, solvents, reaction conditions and yields used in Examples 2 to 16 are shown in Table 1.
[0059] Examples two to sixteen show solvent-free or toluene, chloroform, p-xylene, 1,4-dioxane, 1,2-dichloroethane, carbon tetrachloride, tetrahydrofuran, nitrobenzene or O-dichlorobenzene can be used as a solvent for the reaction; the catalyst is the most ideal formamide series compound.
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