Organic Process Research & Development · 2003 · 109 citations · 14 references
EngineeringOrganic ChemistryPd-catalyzed ReactionsChemistryHeterocycle ChemistryChemical EngineeringMedicinal ChemistryPractical SynthesisResidual PalladiumOrganometallic CatalysisCross-coupling ReactionNew Antimitotic AgentCatalysisPharmacologyAsymmetric CatalysisEnantioselective SynthesisAlkene MetathesisPalladium RemovalNatural SciencesSynthetic Chemistry
A concise large-scale synthesis of 1, a new antimitotic agent is described. The key step was a one-pot Sonogashira cross-coupling of an aryl halide with a heteroaryl halide through an acetylene using the readily available 2-methyl-3-butyn-2-ol (7). An innovative approach for palladium removal was designed and successfully scaled-up on a multikilogram scale. The product was crystallized from the crude reaction mixture while keeping the residual palladium in the mother liquor by using Pd-scavenging agents such as N-acetylcysteine or thiourea.
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Yasushi Nishihara, Kazutaka Ikegashira, Kazunori Hirabayashi et al. · The Journal of Organic Chemistry · 2000 · 271 citations
Chemical Engineering, Disubstituted Ethynes, Engineering +13
One-Pot Palladium-Catalysed Synthesis of Diarylalkynes
Adriano Carpita, Alessandro Lessi, Renzo Rossi · Synthesis · 1984 · 100 citations