Method for preparing organic phosphate compounds from P(O)-OH compounds and methyl-containing substituted aromatic hydrocarbons
A technology of methyl aromatic hydrocarbons and organophosphoric acid, applied in organic chemistry, chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, etc., can solve the problems of cross-substrate applicability, cumbersome experimental steps, and harsh reaction conditions etc. to achieve high selectivity, simple method, and simple preparation
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Embodiment 1
[0028] 109 mg (0.5 mmol) of diphenylphosphoric acid, 105.7 uL (1 mmol) of toluene, 0.1 mmol of catalyst (tetrabutylammonium iodide, tetrabutylammonium bromide, 18-crown-6-ether, iodine ) and 200uL (1.5 mmol) tert-butyl hydroperoxide were added to the Schlenk tube under the air environment, and 0.5 mL toluene was added under the air condition, at 80 o C stirred the reaction for 12 hours. Through GC detection and analysis, when toluene is used as the reaction solvent and only tetrabutylammonium iodide is used as the catalyst, the yield of the crosslinking reaction can reach 67% yield.
Embodiment 2
[0030] Add 109 mg (0.5 mmol) of diphenylphosphoric acid, 105.7 uL (1 mmol) of toluene, 18.5 mg
[0031] (0.1 mmol) tetrabutylammonium iodide and 1.0 mmol oxidant (tert-butyl hydroperoxide, potassium persulfate, hydrogen peroxide, tert-butyl peroxybenzoate, m-chloroperoxybenzoic acid, di-tert-butyl Peroxide, potassium monopersulfate) was added to the Schlenk tube under the air environment, and 0.5 mL of organic solvent toluene was added under the air environment, at 80 o C stirred the reaction for 12 hours. Through GC detection and analysis, when toluene is used as the reaction solvent and only tert-butyl hydroperoxide is used as the oxidant, the yield of the crosslinking reaction can reach 67% yield.
Embodiment 3
[0033]Mix 109 mg (0.5 mmol) of diphenylphosphoric acid, 105.7 uL (1 mmol) of toluene, 18.5 mg (0.1 mmol) of tetrabutylammonium iodide with different molar ratios of tert-butyl hydroperoxide (2.0-6.0 times) into the Schlenk tube under the air environment, add 0.5 mL organic solvent toluene under the air environment, at 25~80 o C stirred the reaction for 12 hours. Through GC detection and analysis, when toluene is used as the reaction solvent, when the consumption of tert-butyl hydroperoxide is 3 times, the yield of the crosslinking reaction can reach 76% yield.
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