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| A novel and green method for the synthesis of 5-bromo-3-phenyl-1, 2, 4-oxadiazole |
| Zhang Weiliang1, Liang Fanghui2, Yue Lin2, Zhang Wenying2, Yu Tonglin2, Wang Juan2 |
1. North China Pharmaceutical Corporation Ltd., Shijiazhuang 052165, China；
2. Shijiazhuang Chemical Fiber Technology Innovation Center of Shijiazhuang University, Shijiazhuang 050035, China |
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Abstract According to the structural characteristics of 1, 2, 4-oxadiazole compounds, 5-bromo-3-phenyl-1, 2, 4-oxadiazole was prepared from benzonitrile through oximation, cyclization, chlorination and bromination. In the synthesis route, the intermediates of the first three steps reaction were synthesized by the conventional methods, and the bromination reaction conditions of the forth step was microwave radiation. The technological parameters involved in microwave reaction were optimized, the structures of the target compound and the intermediates were confirmed by 1H NMR and MS. The results showed that 5-chloro-3-phenyl-1, 2, 4-oxadiazole reactes with trimethylsilyl bromide under 200 W microwave power, 150 ℃ for 15min to give the title compound in 78.2%, and the total yield of the product was 60.0%.
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