Novel synthesis method for phosphate compounds
A technology of phosphate esters and compounds, applied in the field of chemical synthesis, to achieve the effect of large-scale production, cheap raw materials, and easy large-scale production
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Embodiment 1
[0035] In a clean and dry 50ml Schlenk reaction tube, sequentially add 2mmol of 1-phenylethanol, 1mmol of diethyl phosphite, 0.2mmol of cobalt acetate, and 0.2mmol of N-hydroxyphthalimide, and then in the above mixture 5ml of toluene was added as a solvent, the reaction tube was fed with 1 atmosphere of oxygen, the reaction tube was sealed, and the reaction tube was placed in an oil bath at 80° C. for 12 hours. After the reaction, the reaction mixture was directly spin-dried, and the residue obtained was separated by column separation with petroleum ether and ethyl acetate (volume ratio: 2:1). , Phosphorus spectrum analysis, confirmed that the target product was α-diethyl phosphate acetophenone, and the yield was 84%.
[0036] The proton nuclear magnetic resonance spectrum of the product prepared in this embodiment is as follows: Figure 1a As shown, the carbon NMR spectrum is as Figure 1b As shown, the NMR phosphorus spectrum is as Figure 1c shown.
Embodiment 2
[0038] In a clean and dry 50ml Schlenk reaction tube, sequentially add 1mmol of 1-phenylethanol, 1mmol of diethyl phosphite, 0.1mmol of cobalt acetylacetonate, and 0.1mmol of N-hydroxyphthalimide, and then add 6ml of N,N-dimethylformamide was added as a solvent, the reaction tube was fed with 1 atmosphere of oxygen, the reaction tube was sealed, and the reaction tube was placed in an oil bath at 90°C for 18 hours. After the reaction, the reaction mixture was directly spin-dried, and the residue obtained was separated by column separation with petroleum ether and ethyl acetate (volume ratio: 2:1). , Phosphorus spectrum analysis, confirmed that the target product was α-diethyl phosphate acetophenone, and the yield was 75%.
[0039] The proton nuclear magnetic resonance spectrum of the product prepared in this embodiment is as follows: Figure 1a As shown, the carbon NMR spectrum is as Figure 1b As shown, the NMR phosphorus spectrum is as Figure 1c shown.
Embodiment 3
[0041] In a clean and dry 50ml Schlenk reaction tube, sequentially add 2mmol of 1-(4-bromophenyl)-ethanol, 1mmol of diethyl phosphite, 0.2mmol of cobalt acetate, and 0.1mmol of N-hydroxyphthalimide , and then add 6ml of N,N-dimethylformamide as a solvent to the above mixture, inject 1 atmosphere of oxygen into the reaction tube, seal the reaction tube, and place it in an oil bath at 90°C for 15 hours to react. After the reaction, the reaction mixture was directly spin-dried, and the residue obtained was separated by column separation with petroleum ether and ethyl acetate (volume ratio: 2:1). , Phosphorus spectrum analysis, confirmed that the target product was α-diethyl phosphate-4-bromoacetophenone, and the yield was 72%.
[0042] The proton nuclear magnetic resonance spectrum of the product prepared in this embodiment is as follows: Figure 2a As shown, the carbon NMR spectrum is as Figure 2b As shown, the NMR phosphorus spectrum is as Figure 2c shown.
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