用于医药相关合成研究,具体应用场景参考Tetrahedron Letters、Organic Letters等文献报道的相关研究。
医药研究
合成路线 1(1. 合成:40232-88-0)
产率:74%
合成条件:Stage #1: With 3-chloro-benzenecarboperoxoic acid In dichloromethane; water at 0℃; for 7.50 h; Inert atmosphere Stage #2: at 20℃; for 1 h; Inert atmosphere
实验步骤:在氩气氛下,在0°下将间氯过苯甲酸(含有约30%水,纯度> 65%,41.7g,约157mmol)分批加入到S6(25.3g,105mmol)的二氯甲烷(160mL)溶液中。搅拌7.5小时后,将反应混合物用饱和NaHCO 3水溶液淬灭。将混合物用水稀释,分离有机层。用二氯甲烷萃取水层。将合并的萃取液用饱和NaHCO 3水溶液,水和盐水洗涤,用Na 2 SO 4干燥并蒸发。将残余物溶于甲醇(300mL)中,并将K 2 CO 3(72.3g,523mmol)分批加入溶液室温。搅拌1小时后,将混合物减压蒸发。将水加入到残余物中,用乙醚萃取产物。萃取液用水和盐水洗涤,用Na 2 SO 4干燥并蒸发。残余物用二乙醚 - 己烷重结晶,得到浅黄色颗粒状的S7(14.7g,61%)。将上述重结晶的母液蒸发,并将残余物在60N硅胶(己烷 - 乙酸乙酯= 3:1)上进行色谱分离,得到另外的浅黄色固体状的S7(3.14g,13%)。 S7的总量为17.8克(74%)。
参考文献:
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