化学合成。
化学合成
合成路线 1(1. 合成:63558-65-6)
产率:88%
合成条件:With oxalyl dichloride; N,N-dimethyl-formamide In 1,2-dichloro-ethane for 3 h; Heating / reflux
实验步骤:在0℃下向含有7.7mL(99MMOL)DMF和150mL二氯乙烷的搅拌溶液中缓慢加入12.7mL(144.6MMOL)OXALYL氯化物以控制剧烈的气体逸出。 停止放出气体后,加入10.0g碘嘧啶酮,将反应混合物加热回流3小时,然后冷却至室温,在水和二氯甲烷之间分配。 将有机层用MGSO 4干燥,减压除去溶剂,得到9.6g(88%)标题化合物。 1H-NMR(300MHz,CDCl3)A 8.89(s,1H)和8.98(s,1H); ESIMS:241.1(M + H)+
参考文献:
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