化学合成。
化学合成
合成路线 1(1. 合成:21594-52-5)
产率:92%
合成条件:With N-Bromosuccinimide In N,N-dimethyl-formamide at 40℃; for 14 h; Autoclave; Large scale
实验步骤:在干燥的3000mL单颈圆底烧瓶中,加入1500mL乙腈和360mL乙酸,然后加入42. 8g 2,3-二氢吡啶并[2,3-d] [1, 3]酮。完全溶解后,分批加入64.2g NBS(N-溴代琥珀酰亚胺),将反应混合物在室温下搅拌14小时。通过TLC和GC确认反应完成后,加入20mL过二硫酸钠(24g)。通过旋转蒸发除去溶剂,向反应烧瓶中加入300mL水,用300mL乙基萃取混合物两次。合并有机相,用180mL 2N氢氧化钠洗涤,然后用300mL饱和盐水洗涤。用无水硫酸钠干燥过夜。过滤除去硫酸钠,减压蒸发得到粗产物。得到64.1g粗产物,为粗产物,6-溴-3H-恶唑烷[4,5-B]。粗产物用二氯甲烷和乙酸乙酯重结晶,得到纯产物6-溴-3H-恶唑并[4,5-b]吡啶-2-酮59.9g,收率89%。 2%(GC)。熔点231℃至234℃(文献232℃~233℃)。
参考文献:
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