Method for constructing thio (seleno) phosphate ester compound through electrochemical hydrogen desorption oxidative coupling
A technology of hydrogen oxyhydroxide and phosphoric acid ester, applied in the direction of electrolytic components, electrolytic process, electrolytic organic production, etc., can solve the problems of non-conforming to green chemistry, unfriendly environment, low atom economy, etc., and achieve good compatibility and reduce The effect of cost and low energy consumption
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Embodiment 1
[0053]
[0054] Add ethanol (0.5mL) to the reaction tube under nitrogen atmosphere, S 8 (16 mg, 0.5 mmol), diphenylphosphine (89 μL, 0.5 mmol), KI (16.7 mg, 20 mol%) and acetonitrile (10 mL); a carbon rod was used as the anode, and a platinum sheet was used as the cathode. The mixture was stirred at 35° C. for 4 hours under a constant current of 10.0 mA. At the end of the reaction, the solvent was spin-dried under reduced pressure, and the product was purified by silica gel column chromatography to obtain compound 4aa as a yellow solid with a yield of 72%.
[0055] The characterization data of this compound are as follows: 1 H NMR (400MHz, Chloroform-d) δ7.97–7.89(m,4H),7.52–7.42(m,6H),4.14(dq,J=8.8,7.1Hz,2H),1.42–1.23(m,3H ). 13 C NMR (101MHz, Chloroform-d) δ134.71(d, J=110.4Hz), 131.83(d, J=3.0Hz), 131.17(d, J=11.3Hz), 128.46(d, J=13.3Hz) ,61.18(d,J=5.7Hz),16.31(d,J=8.0Hz). 31 P NMR (162MHz, Chloroform-d) δ81.02.
Embodiment 2
[0057]
[0058] Add n-butanol (0.5 mL) into the reaction tube under nitrogen atmosphere, S 8 (16 mg, 0.5 mmol), diphenylphosphine (89 μL, 0.5 mmol), KI (16.7 mg, 20 mol%) and acetonitrile (10 mL); a carbon rod was used as the anode, and a platinum sheet was used as the cathode. The mixture was stirred at 35° C. for 4 hours under a constant current of 10.0 mA. At the end of the reaction, the solvent was spin-dried under reduced pressure, and the product was purified by silica gel column chromatography to obtain a colorless liquid compound 4ba with a yield of 72%.
[0059] The characterization data of this compound are as follows: 1 H NMR (400MHz, Chloroform-d) δ7.96–7.88(m,4H),7.55–7.43(m,6H),4.06(dt,J=8.1,6.5Hz,2H),1.80–1.68(m,2H ),1.54–1.41(m,2H),1.01–0.90(m,5H). 13 C NMR (101MHz, Chloroform-d) δ134.70(d, J=110.4Hz), 131.79(d, J=3.0Hz), 131.18(d, J=11.3Hz), 128.44(d, J=13.3Hz) ,64.71(d,J=5.9Hz),32.38(d,J=7.9Hz),19.02,13.73. 31 P NMR (162MHz, Chloroform-d) δ80.91.
Embodiment 3
[0061]
[0062] Add cyclohexylmethanol (0.5mL) to the reaction tube under nitrogen atmosphere, S 8 (16 mg, 0.5 mmol), diphenylphosphine (89 μL, 0.5 mmol), KI (16.7 mg, 20 mol%) and acetonitrile (10 mL); a carbon rod was used as the anode, and a platinum sheet was used as the cathode. The mixture was stirred at 35° C. for 4 hours under a constant current of 10.0 mA. At the end of the reaction, the solvent was spin-dried under reduced pressure, and the product was purified by silica gel column chromatography to obtain yellow liquid compound 4ca with a yield of 60%.
[0063] The characterization data of this compound are as follows: 1 H NMR (400MHz, Chloroform-d) δ7.96–7.88(m,4H),7.54–7.43(m,6H),3.83(t,J=6.8Hz,2H),1.89–1.66(m,5H), 1.36–1.14(m,4H),1.03(qd,J=12.1,3.4Hz,2H). 13 C NMR (101MHz, Chloroform-d) δ134.67(d, J=110.4Hz), 131.76(d, J=3.0Hz), 131.20(d, J=11.3Hz), 128.42(d, J=13.3Hz) ,69.76(d,J=6.3Hz),38.40(d,J=8.1Hz),29.59,26.41,25.69. 31 P NMR (162MHz, Chloroform-d) δ...
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