医药中间体丙酮缩氨基脲合成研究

Study on Synthesis of a Medicine Intermediate——Acetone Semicarbazone

以水合肼、尿素、丙酮为原料,直接反应合成丙酮缩氨基脲,分别研究了反应温度、反应时间、原料配比、溶剂用量等条件对合成反应的影响,确定了最佳工艺条件。该方法合成丙酮缩氨基脲的最佳工艺条件是:水合肼和尿素反应温度100℃,反应时间7 h;氨基脲与丙酮反应温度55℃,反应时间2 h;n(水合肼)∶n(尿素)∶n(丙酮)=1∶1.6∶3。丙酮缩氨基脲的收率达到97.19%,产品纯度达到98.5%。

Acetone semicarbazone was directly synthesized from hydrazine hydrate, urea and acetone. The effect of reaction temperature, reaction time, materials ratio and the amount of solvent on the synthesis was studied. The proper reaction conditions were as follows：the reaction temperature for hydrazine hydrate and urea was 100℃ and the reaction time was 7 h; the reaction temperature for semicarbazide and acetone is 55 ℃ and the reaction time was 2 h; the molar ratio of hydrazine hydrate：urea：acetone was 1：1.6：3. The yield of the product was 97.19 %, and the purity of acetone semicarbazone was 98.5 % .