化学合成。
医药; 农药; 光电材料
合成路线 1(1. 合成:287192-97-6)
产率:88%
合成条件:With potassium carbonate In methanol at 20℃;
实验步骤:在0℃,向搅拌的4-甲酰基 - 哌啶-1-羧酸叔丁酯(358mg,1.68mmol)和碳酸钾(464mmol,3.36mmol)在甲醇(16ml)中的混合物中滴加a (1-重氮-2-氧代 - 丙基) - 膦酸二甲酯(323mg,1.68mmol)的甲醇(2ml)溶液。 将所得混合物在室温下搅拌过夜,过滤并浓缩。 将残余物在硅胶上进行色谱分离,用乙酸乙酯的己烷溶液(1:5)洗脱,得到标题化合物(308mg,88%),为无色晶体。 LCMS m / e(154,M-M3u + 2H)。 (J. Am.Chem.Soc.2003,125,3714。)
参考文献:
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