Organic Process Research & Development · 2012 · 33 citations · 9 references
Natural SciencesChemistryMedicinal ChemistryDrug DiscoveryGreen ChemistryOrganic ChemistryHeterocyclic ChemistryNatural Product Drug DiscoveryOrganic SynthesisSafer Chemical SynthesisDownstream Processing RobustnessMedicinal Chemistry ApplicationsRearrangement TechniquesSustainable SynthesisYielding
The discovery and development of an efficient and more sustainable manufacturing route to the anti-pneumocystic agent atovaquone (2-((1 R,4 R )-4-(4-chlorophenyl)cyclohexyl)-3-hydroxynaphthalene-1,4-dione) 1 is described. The existing commercial route to atovaquone delivers a poor yield of product and uses expensive reagents. The new synthesis commences with readily available phthalic anhydride, which is converted to 1,4-isochromandione 5 and then to atovaquone 1 by reaction with 4-(4-chlorophenyl)cyclohexanecarboxylic acid 3 using key bromination, Rosenmund reduction, and rearrangement chemistries. Downstream processing to atovaquone is both high yielding and robust, and the resulting process has been demonstrated on 200-kg scale. The process is simple, uses cheap raw materials, and is more sustainable in that it avoids low-yielding silver-promoted chemistry and isomerisation procedures. It includes a robust, facile, and highly efficient procedure to 1,4-isochromandione 5, and routes to 4-(4-chlorophenyl)cyclohexanecarboxaldehyde 9 have also been developed, including a Rosenmund method that was demonstrated on pilot-plant scale. Also discussed are the route-derived impurities and processing amendments to control their formation.
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Synthesis and Anticancer Activities of Novel 1,4-Disubstituted Phthalazines
Juan Li, Yanfang Zhao, Xiaoye Yuan et al. · Molecules · 2006 · 154 citations · Full text
David R. Williams, Michael P. Clark · Tetrahedron Letters · 1998 · 33 citations
Synthesis and in vitro cytotoxicity of novel 1,4-disubstituted phthalazines
Xin Zhai, Juan Li, Lei He et al. · Chinese Chemical Letters · 2007 · 27 citations