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Mechanosynthesis of Odd‐Numbered Tetraaryl n cumulenes
The synthetic approach towards tetraaryl 3 cumulenes 4 encompasses the mechanochemical activation of ketones calcium carbide and potassium hydroxide through a Favorskii alkynylation‐type reaction in a ball mill followed by the establishment of a solventless and acid‐free SnCl 2 ‐mediated reductive elimination of propargylic diols 2 .
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For subsurface injection a powdered carbide is manufactured by ball milling selected sizes of carbide to less than 140 US-mesh (<105 microns). The milled carbide can then be custom blended with a wide range of other powder additives such as lime limestone and
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In a typical synthesis the powders of calcium carbide (CaC 2) and cyanuric chloride (C 3Cl 3N 3) are placed into a 45 mL zirco-nia grinding bowl with 22 zirconia milling balls (d = 10 mm ∼75.7 g). After milling at 500 rpm for a certain time and a con-secutive washing step
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of ball milling techniques.The synthetic approach towards tetraaryl 3 cumulenes 4 encompasses the mechanochemical Scheme 4. Mechanosynthesis of propargylic diols 2a–j and propargyl alcohols 3a–j using calcium carbide. a Yields in parenthesis corre-spond to five-fold scale-up experiments using a45mLZrO2 milling vessel. Scheme 5.
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