产量(工程)
化学
奈韦拉平
叠氮化钠
组合化学
色谱法
二聚体
过程(计算)
钠
三乙醇胺
基础(拓扑)
高效液相色谱法
溶剂
剥离(纤维)
喹啉
作者
Maksim P. Vasilev,Rajasekar Reddy Annapureddy,Chengfeng Ye,Sridhar Regati,Praveen Kumar Gajula,Jonathan M. Bietsch,Zhirui Wang,Jack D. Brown,Gopal Sirasani,Aravind S. Gangu,Paul Guo,Bo Qu,Chris H. Senanayake
标识
DOI:10.1021/acs.oprd.6c00277
摘要
Abstract A telescoped two-step fully continuous-flow process for the synthesis of nevirapine (trade name: Viramune), a key therapeutic agent for the prevention and treatment of HIV-1 infection, has been developed. The process employs, for the first time, sodium bis(trimethylsilyl)amide (NaHMDS) as a homogeneous, process-friendly base for both reaction stages and enables direct conversion of methyl 2-(cyclopropylamino)nicotinate and 2-chloro-3-amino-4-picoline to nevirapine without isolation of the cyclization intermediate. The optimized process operates with a total residence time of 10 min and delivers crude nevirapine in 91.9% overall isolated yield across two reaction steps, with a space-time yield of ∼365 g/h/L and 99.6 A% HPLC purity. Furthermore, we developed an on-demand continuous generation of NaHMDS in diglyme (up to ∼2.0 M) using a sodium packed-bed column reactor. Using on-demand generated NaHMDS, the telescoped synthesis yielded crude nevirapine in 90.7% isolated yield (∼340 g/h/L space-time yield and 99.5 A% purity), providing a scalable and cost-effective alternative to NaH applied in the current commercial synthesis.
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