化学合成;生命科学。
化学合成;生命科学
合成路线 1(1. 合成:93267-04-0)
产率:68%
合成条件:at 0 - 20℃; for 1.50 h;
实验步骤:将三苯基膦(131g,0.500mol)和咪唑(34g,0.50mol)在DCM(600mL)中的混合物冷却至0℃并在0.5小时内分小份加入碘化物(127g,0.50mol)。 移去冷却浴,将混合物搅拌0.5小时。 将混合物再次冷却至0℃后,滴加(5) - 2 - ((叔丁氧基羰基)氨基)-3-羟基丙酸甲酯(73g,0.33mol)的DCM(300mL)溶液。。 加完后,移去冷却浴,将混合物温热至室温并搅拌1.5小时。 过滤混合物,浓缩滤液以除去大部分溶剂。 将MTBE(400mL)加入到残余物中,过滤混合物以除去三苯基氧化膦。 浓缩滤液,通过硅胶快速柱色谱法纯化残余物,得到(R) - 2 - ((叔丁氧基羰基)氨基)-3-碘代丙酸甲酯(74.0g,68%收率),为无色固体。
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