A novel method for efficiently preparing diarylmethyl-substituted organic phosphonates with p(o)-h compounds
A technology of diarylmethyl and organic phosphonic acid, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve the problem of harsh reaction conditions, raw material quality, safety and product stability And purity problems, difficult synthesis technology and other problems, to achieve the effect of mild and easy to control the reaction process, good industrial application prospects, and cheap and easy-to-obtain catalysts
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Embodiment 1
[0026] 101.1 mg (0.5 mmol) of diphenylphosphine, 176.4 mg (0.6 mmol) of 4-phenylmethylene-2,6-di-tert-butyl-2,5-cyclohexadien-1-one , 0.1 mmol of cesium carbonate, put into the Schlenk tube under nitrogen atmosphere, add 1.0 mL solvent (dichloromethane, dichloroethane, tetrahydrofuran, acetonitrile, methanol, dioxane, toluene, N, N -dimethylformamide), at 40 o The reaction was stirred at C for 6 hours. pass 31 P NMR NMR yield detection analysis, when acetonitrile is used as the solvent, the yield of the 1,6-addition reaction is 99%.
Embodiment 2
[0028] 101.1 mg (0.5 mmol) of diphenylphosphine, 176.4 mg (0.6 mmol) of 4-phenylmethylene-2,6-di-tert-butyl-2,5-cyclohexadien-1-one , cesium carbonate (20 mol%, 10 mol%, 5 mol%, 2 mol%, 1 mol%) was added to the Schlenk tube under nitrogen atmosphere, and added to 1.0 mL of acetonitrile under nitrogen atmosphere, at 40 o The reaction was stirred at C for 6 hours. pass 31 P NMR NMR yield detection analysis, when the amount of cesium carbonate was 5 mol%, the yield of the 1,6-addition reaction was 99%.
Embodiment 3
[0030] 101.1 mg (0.5 mmol) of diphenylphosphine, 176.4 mg (0.6 mmol) of 4-phenylmethylene-2,6-di-tert-butyl-2,5-cyclohexadien-1-one , 5 mol% cesium carbonate, put into Schlenk tube under nitrogen atmosphere, add 1.0 mL of acetonitrile under nitrogen atmosphere, at 25~80 o The reaction was stirred at C for 6 hours. pass 31 P NMR nuclear magnetic yield detection analysis, when the reaction temperature is 40 o C, the yield of the 1,6-addition reaction was 99%.
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