连续搅拌釜式反应器
生物催化
过程(计算)
可扩展性
化学
纳米技术
计算机科学
组合化学
化学工程
材料科学
工程类
有机化学
催化作用
反应机理
数据库
操作系统
作者
Qiang Yang,Yu Lu,Thomas J. Beauchamp,Kevin P. Cole,Jiang Wang,Srinivas Gangula,Silong Zhang,Zhaoshan Cui,Guopeng Wang,Lei Shi,Dajiang Jing,Fuliang Wei,Xuecheng Jiao,Xiang Li,Na Zhang,Xiangjun Jiang,Yulei Ma
标识
DOI:10.1021/acs.oprd.5c00003
摘要
Process development and scale-up of the synthesis of a pyridazinyl imidazolidinone intermediate for the production of an imidazo[1,2-b]pyridazine IL-17A inhibitor are described. A transamination process was developed for the preparation of (S)-3,3,3-trifluoropropane-1,2-diamine, eliminating an unstable enamine intermediate that significantly limited the scalability of the original asymmetric hydrogenation route. A CSTR continuous flow process was developed for the carbonylation of N-(6-chloropyridazin-3-yl)pivalamide under cryogenic conditions that successfully suppressed product decomposition, improving the isolated yield to ∼60% from the ∼40% yield of the batch mode process. A robust KRED process was developed for the reduction of N-(6-chloro-5-(2-methoxyacetyl)pyridazin-3-yl)pivalamide to the corresponding chiral alcohol, which was further derivatized as its triflate for the SN2 reaction with (S)-3,3,3-trifluoropropane-1,2-diamine and treated with carbonyl diimidazole to assemble the target pyridazinyl imidazolidinone intermediate. The developed process was successfully scaled up to deliver 157 kg of the pyridazinyl imidazolidinone intermediate to support the production of the final drug substance, demonstrating the robustness of the optimized process.
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