以双标记13C,15N3 -氨基脲为原料,先与苯甲醛缩合,继而与氯乙酸乙酯取代、环化,再经盐酸水解反应后与5-硝基糠醛二乙酯反应,最终制得双标记13C,15N3-呋喃妥因.产物经红外光谱、高效液相色谱及质谱表征.结果表明,所选用的合成路线反应条件温和,产物总收率高于60％,且同位素丰度不下降；目标产物的化学纯度＞99.0％,13C同位素丰度＞98％,15N同位素丰度＞99％.%A novel method was established to synthesize double labeled 13C,15N3-nitrofurantoin. Starting material 13C,15 N3-semicarbazide was firstly converted to benzaldehyde semicarbazone (II) by condensation with benzaldehyde. Compound (II) was then allowed to react with ethyl a-chloroacetate in the presence of sodium ethoxide, forming 1-benzylideneaminohydratoin (III). Compound (III) was hydrolyzed with hydrochloric acid and condensed with 5-nitro furfural diacetate, generating the target compound) nitrofurantoin-13C,l5N3) (V). As-synthesized target product was characterized by infrared spectrometry, high-performance liquid chromatog-raphy, and mass spectrometry. It has been found that the established synthetic route is dominated by mild reaction conditions and gives rise to the final product in a yield of above 60%, while the abundance of the isotopes does not tend to decline. Namely, the chemical purity of the target product is above 99. 0%, and the abundances of 13C and 15N are above 98% and 99%, respectively.
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