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With potassium peroxymonosulfate; In d(4)-methanol; water-d2; at 20℃; for 5h;
General procedure: To an NMR tube, 8.4 mg (50 μmoles) of 1 and 2.2 mg (30 μmoles) of tBuOH (used as an internal standard) in a 750 μL solution of 10% (v/v) d3-ACN in D2O were added. A 1H-NMR spectrum was recorded as a zero point (time = 0). A stock solution of 400 mM Oxone in 10% (v/v) d3-ACN in D2O was prepared and a 250 μL aliquot of the Oxone solution was added to the NMR tube to initiate the reaction. The reaction was followed by 1H-NMR spectroscopy over the course of 5 hrs at room temperature. The yields reported were based on the integration of aromatic peaks against the internal standard. This procedure was repeated for each of the different mol equivalents of Oxone, for the different cosolvents, and substrates.
With potassium peroxymonosulfate; In [D3]acetonitrile; water-d2; at 20℃; for 5h;
General procedure: To an NMR tube, 8.4 mg (50 μmoles) of 1 and 2.2 mg (30 μmoles) of tBuOH (used as an internal standard) in a 750 μL solution of 10% (v/v) d3-ACN in D2O were added. A 1H-NMR spectrum was recorded as a zero point (time = 0). A stock solution of 400 mM Oxone in 10% (v/v) d3-ACN in D2O was prepared and a 250 μL aliquot of the Oxone solution was added to the NMR tube to initiate the reaction. The reaction was followed by 1H-NMR spectroscopy over the course of 5 hrs at room temperature. The yields reported were based on the integration of aromatic peaks against the internal standard. This procedure was repeated for each of the different mol equivalents of Oxone, for the different cosolvents, and substrates.
With potassium peroxymonosulfate; In [D3]acetonitrile; water-d2; tert-butyl alcohol; at 20℃; for 5h;Schlenk technique; Inert atmosphere;
To an NMR tube, 8.4 mg (50 μmoles) of 1 and 2.2 mg (30 μmoles) of tBuOH (used as an internal standard) in a 750 μL solution of 10% (v/v) d3-ACN in D2O were added. A 1H-NMR spectrum was recorded as a zero point (time = 0). A stock solution of 400 mM Oxone in 10% (v/v) d3-ACN in D2O was prepared and a 250 μL aliquot of the Oxone solution was added to the NMR tube to initiate the reaction. The reaction was followed by 1H-NMR spectroscopy over the course of 5 hrs at room temperature. The yields reported were based on the integration of aromatic peaks against the internal standard. This procedure was repeated for each of the different mol equivalents of Oxone, for the different cosolvents, and substrates.
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