节点文献
新型氨基硫脲类Schiff碱配体的合成及结构表征
Synthesis and Characterization of New Schiff Base Type Lig ands Containing Thiosemicarbazide Group
【摘要】 用 0 .0 5mol烯丙基异硫氰酸酯和 9.5mL质量分数为 5 0 %的水合肼溶液反应 ,制得 6 3g新的烃基取代的氨基硫脲类化合物——— 4 烯丙基氨基硫脲 (Ⅰ)白色晶体。首先用 0 0 1mol联乙酰分别与 0 0 2mol化合物Ⅰ及 0 0 2mol氨基硫脲缩合 ,合成了收率为 71%的联乙酰双缩 ( 4 烯丙基氨基硫脲 ) (Ⅱ)和收率为 70 %的联乙酰双缩氨基硫脲 (Ⅲ)两种新的含硫脲基Schiff碱。其次用 10mmol环己酮与 10mmol化合物Ⅰ在 30mL无水乙醇中 ,电磁搅拌 ,回流反应 2h ,合成出 1 8g环己酮缩烯丙基氨基硫脲 (Ⅳ )淡黄色晶体。最后将 0 0 1mol化合物Ⅰ分别与 0 0 0 5mol水合茚三酮及 1 0g乙二醛缩合 ,合成了两种新的含硫脲基的双Schiff碱型配体——— 1 6g茚三酮二缩 ( 4 烯丙基氨基硫脲 ) (Ⅴ)桔红色晶体和 1 2g乙二醛二缩 ( 4 烯丙基氨基硫脲 ) (Ⅵ )浅黄色粉末。对所合成的 5种新的含硫脲基Schiff碱配体 ,通过元素分析 ,IR ,1HNMR和MS表征了它们的结构。初步测试了它们对部分金属离子的配位性能。该合成方法具有操作简便、反应条件温和、产率高等优点
【Abstract】 Allylthiosemicarbazide(Ⅰ),prepared from allyl iso thiocyanate and hydrazine, reacted with butane-2,3-dione,ninhydrin,or glyoxal to give butane-2,3-dione bis-(4-allylthiosemicarbazone) (Ⅱ),ninhydrin-1,3-bis(4-allylthiosemicarbazone) (Ⅴ),or glyoxal bis(4-ally lthiosemicarbazone)(Ⅵ) respectively.Butane-2,3-dione bis-thiosemicarbazone( Ⅲ) was obtained via the reaction of butane-2,3-dione and aminothiourea.Cyclohexanone 4-allylt hiosemicarbazone (Ⅳ) was also prepared.The structures of these compounds were c onfirmed by elemenmtary analysis,IR, 1H-NMR and MS spectra.Their complexati on behaviors with some metal ions were preliminarily determined under different conditions.Compared with classical synthetic methods, this one has the advantage s of simple operation,mild conditions and high yields.
【Key words】 Schiff base type ligand containning thiosemicarba zide; 4-allylthiosemicarbazide; allyl isothiocyanate;
- 【文献出处】 精细化工 ,FINE CHEMICALS , 编辑部邮箱 ,2000年10期
- 【分类号】O627
- 【被引频次】14
- 【下载频次】369