化学合成。
医药; 化工
合成路线 1(1. 合成:885518-82-1)
产率:93.3%
合成条件:With iodine; potassium hydroxide In N,N-dimethyl-formamide at 0 - 20℃; for 1 h;
实验步骤:在0℃下向26-S1(2.5g,14.2mmol)的DMF(30mL)溶液中分批加入KOH(1.8g,31.9mmol,然后分别加入碘(5.4g,21.3mmol)。反应混合物为 在室温下搅拌1小时。将反应混合物倒入冰水中,用EtOAc萃取两次。合并的有机物用5%Na 2 S 2 O 4水溶液和盐水洗涤,干燥,浓缩至干,得到26-S2(4.0g, 得到93.3%产率,为黄色固体,其不经进一步纯化直接在下一合成步骤中进行.LC / MS(ESI)m / z:303(M + H)+。
参考文献:
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