二苯基甘脲的简便合成及表征

Simple Synthesis and Characterization of Diphenylglycoluril

以安息香为原料经氧化制得联苯偶酰,再与脲缩合生成二苯基甘脲。考察了缩合反应的影响因素。结果表明,以无水乙醇为溶剂,乙醇钠为催化剂,在室温下即可反应,当脲与联苯偶酰投料摩尔比为2.5∶1,催化剂用量为联苯偶酰物质的量的10%时,40℃下,反应1.5 h,二苯基甘脲平均收率为82%。对产物进行了IR、1HNMR、13CNMR及HPLC-MS表征,HPLC色谱纯度为98%。

Diphenylglycoluril was synthesized by condensation reaction of urea with dibenzoyl that was produced through the oxidation of benzoin. The results show that,with anhydrous ethanol as solvent,sodium ethoxide as catalyst,the condensation reaction began at room temperature; under the conditions of the molar ratio of 2. 5∶1of urea and dibenzoyl,the dosage of catalyst 10% of dibenzoyl,40 ℃,1. 5 h,the average yield of diphenylglycoluril was 82%. The product was analyzed and characterized by means of IR,1HNMR,13 CNMR and HPLC-MS,and the purity was 98% by HPLC.