光谱学与光谱分析 |
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Monitoring the Synthesis of N,N-Diphenyl Urea by IR-Online |
YAO Jie, KANG Tao, HU Xiao-jia, CHEN Tong*, LEI Yong-cheng, WANG Gong-ying* |
Chengdu Institute of Organic Chemistry,Chinese Academy of Sciences,Chengdu 610041, China |
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Abstract IR-online detector, React IRTM 4000, was used to monitor the synthesis of N,N-diphenyl urea from urea and aniline. The concentration changes of the reaction components were obtained according to the characteristic IR absorbance changes of the reactants (urea and aniline) at 1 420 and 1 270 cm-1 respectively, the intermediate product (monophenylurea) at 1 339 cm-1 as well as the product (N,N-diphenyl urea) at 1 312 cm-1. In the present study, the result showed that the synthesis of N,N-Diphenyl urea was carried out by two steps. Firstly, the intermediate product monophenylurea was synthesized from urea and aniline, and then N,N-diphenyl urea was obtained by the reaction of monophenylurea with aniline. It was also shown that the IR-online detector was a fast, simple and exact technique to optimize the reaction time and so the reaction course could be easily controlled. The result of IR-online spectrometry was approved by offline reference high performance liquid chromatography (HPLC) method. As a result, the IR-online spectrometry was superior to HPLC method since it was a nondestructive method without the need to sample the reaction medium.
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Received: 2008-05-12
Accepted: 2008-08-16
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Corresponding Authors:
CHEN Tong,WANG Gong-ying
E-mail: chentongw@sina.com.cn
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