Abstract
Using Schiff base as a phase transfer catalyst, ethoxycarbonyl isothiocyanate was synthesized by reacting ethyl chloroformate with sodium thiocyanate. In order to get the best synthetic technology, an orthogonal test (L 9(34)) was applied. The results show that reaction temperature, reaction time, content of catalyst and molar ratio of sodium thiocyanate to ethyl chloroformate are the main factors influencing the yield. The four factors chosen for the present investigation are based on the results of a single-factor test. The optimum synthetic technology is determined as follows: reaction temperature 35 °C, reaction time 3 h, the content of catalyst (molar fraction based on ethyl chloroformate) 1.5% and molar ratio of sodium thiocyanate to ethyl chloroformate 1.1. Under the optimized synthetic technology, the experimental yield reaches 96.8%.
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Foundation item: Project(2007AA06Z122) supported by the National High Technology Research and Development Program of China; Project(20110491267) supported by the Postdoctoral Science Foundation of China; Project(74341015502) supported by Postdoctoral Fund of Central South University, China
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Liang, wj., Zhong, H. & He, Mh. Synthesis of ethoxycarbonyl isothiocyanate by orthogonal design. J. Cent. South Univ. 19, 2447–2450 (2012). https://doi.org/10.1007/s11771-012-1295-8
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DOI: https://doi.org/10.1007/s11771-012-1295-8