活性成分
化学
吡啶
酒石酸盐
产量(工程)
氯
再结晶(地质)
成分
有机化学
过程开发
组合化学
对映体
吡啶
药品
制造工艺
作者
Joseph Ryan,Aida Ajaz,Rajender Vemula,Christopher R. H. Hale,Giorgio Attardo,MVRCH Murthy,Yolanda Gasanz,Vijaya Bhasker Gondi
标识
DOI:10.1021/acs.oprd.6c00185
摘要
Development of the commercial manufacturing strategy and process employed for xanomeline tartrate ( KTX-001), a key active pharmaceutical ingredient (API) in KarXT, is described. The development process involved identifying efficient processes for key bond-forming steps, including the conversion of regulatory starting material nicotinaldehyde ( 1 ) to stage 1 regulatory intermediate chlorothiadiazole 2, nucleophilic aromatic displacement of the chlorine atom within 2 with 1-hexanol followed by methylation to generate stage 2 regulatory intermediate pyridinium 4, and selective partial reduction of the pyridine ring to produce the API freebase, which after tartrate salt formation gave access to stage 3 regulatory intermediate crude xanomeline tartrate ( crude KTX-001 ). A recrystallization process was developed to provide the drug substance xanomeline tartrate ( KTX-001 ) in an overall yield of 35% from nicotinaldehyde ( 1 ) with HPLC purity of >99.0% on scales of 500+ kilograms per batch, suitable for reliable supply of this commercial drug substance.
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