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Radical Oxidation of Allylic and Benzylic Alcohols01:21

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Activated manganese(IV) oxide can selectively oxidize allylic and benzylic alcohols via a radical intermediate mechanism. Primary allylic alcohols are oxidized to aldehydes, while secondary allylic alcohols yield ketones. The redox reaction of potassium permanganate with an Mn(II) salt such as manganese sulfate (under either alkaline or acidic conditions), followed by thorough drying, yields the oxidizing agent: activated MnO2. While MnO2 is insoluble in the solvents used for the reaction, the...
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Diols are compounds with two hydroxyl groups. In addition to syn dihydroxylation, diols can also be synthesized through the process of anti dihydroxylation. The process involves treating an alkene with a peroxycarboxylic acid to form an epoxide. Epoxides are highly strained three-membered rings with oxygen and two carbons occupying the corners of an equilateral triangle. This step is followed by ring-opening of the epoxide in the presence of an aqueous acid to give a trans diol.
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Oxidation of Alcohols02:37

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The oxidation of an organic compound in the presence of air or oxygen is called autoxidation. For example, cumene reacts with oxygen to form hydroperoxide. Autoxidation involves initiation, propagation, and termination steps. Many organic compounds are susceptible to autoxidation—especially ethers in the presence of oxygen, which form hydroperoxides. Even though this reaction is slow, old ether bottles contain small amounts of peroxide, which leads to laboratory explosions during ether...
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Alkenes are converted to 1,2-diols or glycols through a process called dihydroxylation. It involves the addition of two hydroxyl groups across the double bond with two different stereochemical approaches, namely anti and syn. Dihydroxylation using osmium tetroxide progresses with syn stereochemistry.
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Verónica Pinos-Vélez1,2,3, Oscar Osegueda1,4, Dana Georgiana Crivoi1

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Understanding catalyst deactivation is crucial. Small palladium (Pd) clusters and single atoms on corundum, prepared by impregnation, maintain activity during hydrogen cycles, unlike larger Pd nanoparticles.

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Area of Science:

  • Materials Science
  • Catalysis
  • Surface Chemistry

Background:

  • Catalyst deactivation mechanisms are critical for developing efficient and durable catalysts.
  • Palladium (Pd) supported on corundum (Al2O3) is a widely studied catalytic material.

Purpose of the Study:

  • To investigate the behavior of Pd/corundum catalysts during hydrogen adsorption/desorption cycles.
  • To elucidate the role of different Pd species (nanoparticles, clusters, single atoms) in catalyst deactivation.

Main Methods:

  • Temperature-programmed desorption coupled with mass spectrometry (TPD-MS).
  • Aberration-corrected transmission electron microscopy (AC-TEM).
  • Preparation of Pd/corundum by impregnation and sputtering.

Main Results:

  • Uniformly dispersed Pd nanoparticles were observed in both preparation methods.
  • Single atoms and small Pd clusters were exclusively found in materials prepared by impregnation.
  • Larger Pd nanoparticles (>2 nm) transformed into a Pd/PdHₓ core-shell structure upon hydrogen exposure.
  • Pd nanoparticles <2 nm and single atoms remained unchanged.

Conclusions:

  • The long-term activity of Pd/corundum catalysts prepared by impregnation is attributed to the stability of small Pd clusters and single atoms.
  • Understanding the deactivation of larger Pd nanoparticles is key to improving catalyst longevity.