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All reagents and solvents were pure analytical grade materials purchased from commercial sources and were used without further purification, if not stated otherwise. All melting points are uncorrected. The NMR spectra were recorded in CDCl3 on a Bruker Avance 400 MHz instrument with TMS as internal standard. TLC was carried out with 0.2 mm thick silica gel plates (GF254, The columns were hand packed with silica gel 60 (200-300 μm, All products were confirmed by 1H NMR and 13C NMR. Unknown compounds were additionally confirmed by elemental analysis. Typical Procedure for the Oxidative Amidation of Aldehydes with Amines by DIB: A solution of aldehyde (0.50 mmol, 1.0 equiv, DIB (0.75 mmol, 1.5 equiv, and two drops of H2O in CHCl3 (1 mL) was cooled to 0°C under an inert atmosphere (N2) and the amine (0.65 mmol, 1.3 equiv) was slowly added about one drop in 1 h for 3 h, The reaction vessel was capped and t
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4: C, 61.64; H, 7.56; N, 5.53; O, 25.27. Found: C, 61.60; H, 7.65; N, 5.60.
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54149101749
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- was recovered and recycled in our previous work. Please refer to ref. 12.
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- was recovered and recycled in our previous work. Please refer to ref. 12.
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