629-23-2Relevant articles and documents
Copper-catalyzed method for preparing aldehyde or ketone compound by oxidizing alcohol with oxygen as oxidizing agent and application
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Paragraph 0028-0030; 0160-0162, (2020/08/18)
The invention discloses a copper-catalyzed method for preparing an aldehyde or ketone compound by oxidizing alcohol with oxygen as an oxidizing agent. Reaction is performed in an organic solvent for 4-48 hours at room temperature by using copper salt and nitroxide free radicals as catalysts and oxygen or air as an oxidizing agent to efficiently oxidize an alcohol compound into the corresponding aldehyde or ketone compound. The method is simple to operate, free of chlorides corrosive to equipment, available in raw materials and reagents, mild in reaction conditions, wide in substrate universality, good in functional group compatibility, convenient in separation and purification, environmentally friendly in the whole process and free of pollution, and is a method suitable for industrial production.
A general method for the direct transformation of common tertiary amides into ketones and amines by addition of Grignard reagents
Huang, Pei-Qiang,Wang, Yu,Xiao, Kai-Jiong,Huang, Ying-Hong
, p. 4248 - 4254 (2015/06/02)
The direct transformation of amides into ketones by addition of organometallic reagents has attracted the attention of organic chemists for a long time. However limited methods are reliable for common amides and have found synthetic applications. Here we report a method featuring in situ activation of tertiary amides with triflic anhydride (Tf2O) followed by addition of Grignard reagents. The method displays a good generality in scope for both amides and Grignard reagents, and it can be viewed as the acylation of Grignard reagents using amides as stable and selective acylating agents. Moreover, this deaminative alkylation reaction provides a mild method for the N-Deacylation of amides to give free amines.
Hyperfine Structures of Doxyl-Labeled n-Alkyl Chains by NMR and EPR
Bales, Barney L.,Mareno, Donna,Harris, Francis L.
, p. 37 - 53 (2007/10/02)
The proton hyperfine coupling constants in a series of n-alkyl chains with a doxyl group attached at various points from the end of the chain have been measured by NMR and EPR spectroscopies.The hyperfine structure shows no further change when the attachment point is four or more carbon-carbon bonds from the end of the chain.The high resolution afforded by 500 MHz NMR reveals small magnetic inequivalencies in the chain methylene hyperfine coupling constants located at the same distance from the attachment point.Protons in the same chain methylene group are shown to have different hyperfine coupling constants while protons on different chain methylene groups, symmetrically placed with respect to attachment point, are the same, in every case except one.EPR spectra simulated from hyperfine coupling constants derived from NMR are in excellent agreement with experiment.Inhomogeneous EPR line broadening is found to be in excellent agreement with a previously derived universal hyperfine pattern (B.L.Bales, in "Biological Magnetic Resonance" (L.J.Berliner and J.Reuben, Eds.), Vol. 8, p. 77, Plenum, New York, 1989), so no new correction procedures are necessary.Strategies for selectively deuterating n-alkyl spin probes are developed and compared with some results taken from the literature.Deuterating the chain methylene groups two to three carbon-carbon bonds from the attachment point is necessary for the maximum gain in resolution and sensitivity.
