羰基二咪唑合成工艺的研究

Research in the synthetic method of carbonyldiimidazole

对羰基二咪唑的合成工艺进行了研究。采用咪唑、六甲基二硅胺烷为起始原料,经缩合得到三甲基硅咪唑,然后再与三光气反应得到产物羰基二咪唑。实验考察了三甲基硅咪唑合成过程中的各种影响因素,确定该反应的最佳工艺条件为:咪唑∶六甲基二硅胺烷(摩尔比)=1∶0.6,反应温度为105℃,反应时间为5 h;合成羰基二咪唑的反应配比为:三甲基硅咪唑∶三光气(摩尔比)=7∶1。在该工艺条件下,羰基二咪唑的合成反应总收率可达90.4%,产品纯度为98.5%,并用红外光谱对产物进行结构表征。

A new synthesis of carbonyldiimidazole was researched.The carbonyldiimidazole was synthesized from imidazole and hexamethyl disilyamine through condensation,and then the intermediates reacted with triphosgene.The experiment researched all kinds of effect factors during the synthesis of trimethylsilyl imidazole.It was found that the best reaction conditions were as follows：imidazole ∶hexamethyl disilyamine（mol/mol）=1 ∶0.6,reaction temperature 105 ℃ and reaction time 5 h.The suitable ratio of trimethylsilyl imidazole to triphogene（mol/mol） was 7 ∶1.Under these conditions,its total yield was 90.4% and the purity of product reached 98.5%,the product was characterized by IR.