The final NMR-pure products were obtained by evaporation of Et 2O from the extract most prepared carbonyl compounds were additionally identified as their 2,4-dinitrophenylhydrazones. After completion of the reaction, the solution was extracted with Et 2O. (the reactions were monitored by TLC via disappearance of the alcohol). The reaction mixture was stirred for a period of time indicated in Figures Then, the alcohol (0.1 mmol) and an aqueous solution of RuCl 3 (2.0 µL of 0.25 M solution 0.5 µmol) were added under stirring at r.t. Method B: m-Iodosylbenzoic acid ( 2 40 mg, 0.15 mmol) was added to an aqueous solution of NaHCO 3 (63 mg in 1.0 mL of H 2O) and the mixture was stirred until the formation of a clear solution was observed. m-Iodobenzoic acid ( 1) can be easily regenerated (>95%) from IRA 900 by treatment with aq HCl and reused without additional purification. Most products were additionally identified as 2,4-dinitrophenylhydrazones, prepared by the treatment of reaction mixtures with a standard solution of 2,4-dinitrophenylhydrazine. The polymer was removed by filtration and the solution was concentrated under vacuum to afford the NMR-pure carbonyl compound. Then, CH 2Cl 2 (1.5 mL) and IRA 900 (hydroxide form 160-620 mg) were added and the mixture was stirred for 5 min. An instantaneous formation of a cotton-like, off-white precipitate was observed. Method A: To a mixture of alcohol (0.05-0.20 mmol) and m-iodosylbenzoic acid ( 2 0.075-0.300 mmol, 1.5 equiv) in aq MeCN (MeCN-H 2O, 5:1 0.5-2 mL) an aqueous solution of RuCl 3 (1.0-4.0 µL of 0.25 M solution 0.25-1.0 µmol) was added under stirring at r.t. RuCl 3 -Catalyzed Oxidation of Alcohols to Carbonyl Compounds: The solid was then dried, first by maintaining suction and then in vacuum, to afford product 2 as a light yellow powder. The precipitate was filtered on a Büchner funnel and washed with ice-water (200 mL). The reaction mixture was poured onto ice-water (150 mL), and allowed to crystallize. A spontaneous heating of the reaction mixture up to 45 ☌ and complete dissolution of m-iodobenzoic acid was observed during the first two hours of stirring. Improved Procedure for the Preparation of m -Iodosyl-benzoic Acid ( 2): m-Iodobenzoic acid ( 1 2.48 g, 10 mmol) was added at 40 ☌ to a freshly prepared solution of peracetic acid in AcOH and the resulting mixture was stirred for 12 h at ambient temperature in dark. 1a Hypervalent Iodine Chemistry Wirth T.M-iodosobenzoic acid - oxidation - catalysis - scavenger Machine Learning and Artificial Intelligence in Chemical Synthesis and Catalysis.Design and Chemical Synthesis of Antivirals.Virtual Pearl Anniversary Issue – 30 Years SYNLETT.Virtual India Collection: Most Cited SYNLETT Articles and Related Synthetic Methodology Reviews from Science of Synthesis.20 most-cited SYNLETT articles published in 2019/2020.Editorial Board Collection published in 2020/2021.Nobel Prize 2021 Collection – Ben List and David MacMillan.20 most-cited SYNLETT articles published in 2020/2021.Pearl Anniversary Issue – 30 Years SYNLETT.Special Section: 10th EuCheMS Organic Division Young Investigator Workshop.Electrochemical Synthesis and Catalysis.Organosulfur and Organoselenium Compounds in Catalysis.9th Pacific Symposium on Radical Chemistry.Special Section: 11th EuCheMS Organic Division Young Investigator Workshop.Integrated Synthesis Using Continuous-Flow Technologies.Radicals – by Young Chinese Organic Chemists.Modern Heterocycle Synthesis and Functionalization.The Power of Transition Metals – In Honor of Prof.Perspectives on Organoheteroatom and Organometallic Chemistry.Modern Nickel-Catalyzed Reactions – Part II.Modern Nickel-Catalyzed Reactions – Part I.Special Section: 12th EuCheMS Organic Division Young Investigator Workshop.To view the current address, phone number, age, and associates of any adult in Rockaway, NJ simply click a name listed below. Select a Person in Rockaway, NJ to View Detailsīrowse the list of people in Rockaway, NJ below.
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