1,3-Diphenylurea synthesis
- Product Name:1,3-Diphenylurea
- CAS Number:102-07-8
- Molecular formula:C13H12N2O
- Molecular Weight:212.25
Yield:102-07-8 99%
Reaction Conditions:
Stage #1:bis(trichloromethyl) carbonate;aniline in acetonitrile at 0 - 5; for 1 h;
Stage #2: with ETS-10 molecular sieve catalyst in acetonitrile at 80; for 4 h;Solvent;Temperature;
Steps:
1 Example 1
Taking 0.93g aniline, 1.08g triphosgene in 100 ml reaction tube, add 25 ml acetonitrile, ice-bath (0 - 5 °C) under reaction, TLC tracking detection, about 1 hours the reaction is complete. Then adding 0.09g ETS - 10, raising the temperature to 80 °C continuing to stir, TLC detection, about 4h reaction is complete. After cooling, centrifugal separation, and steaming and recovery acetonitrile solution obtained diphenyl urea solid product 1.05g, melting point m.p. 245.0 - 245.2 °C, yield 99%, purity 99.91% (HPLC detection). Centrifugal solid catalyst, distillation is acetonitrile solvent for repeated reaction, reaction conditions, raw material on the same, repeated 5 times and, yield is 97% or more, to be repeated 6 times and, yield is 92%, the purity of 98% or more.
References:
Wenzhou University;Xiong Jing;Wu Guanghui;Xiang Huabin;Zhao Haiyang;Xu Yangbiao CN104725280, 2017, B Location in patent:Paragraph 0029-0030
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