Refining and purifying method of 2, 2 '-dinitroethylene glycol diphenyl ether

The invention provides a refining and purifying method of 2, 2 '-dinitroethylene glycol diphenyl ether. According to the technical scheme, a synthetic route that o-nitrochlorobenzene and ethylene glycol are used as raw materials and are subjected to an O-alkylation reaction under the catalysis...

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Hauptverfasser: ZHEN MEIJING, ZHANG JUNHONG, LI LI, ZHOU WEIYE, GAO XIHUI, ZHOU-ZI LONGTIAN, LI QIANGYING, TENG XUEJIN, WU XIAOFENG, ZHENG KAIJUN, GENG SHISHU, LIU QINGXUE, LI PEICHENG
Format: Patent
Sprache:chi ; eng
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Zusammenfassung:The invention provides a refining and purifying method of 2, 2 '-dinitroethylene glycol diphenyl ether. According to the technical scheme, a synthetic route that o-nitrochlorobenzene and ethylene glycol are used as raw materials and are subjected to an O-alkylation reaction under the catalysis of a phase transfer catalyst and an alkaline condition is abandoned. O-nitrophenol is adopted as a raw material and reacts with dichloroethane under the catalytic condition, and 2, 2 '-dinitroethylene glycol diphenyl ether is generated in one step. The synthetic route has few side reactions and low impurity content, and lays a foundation for subsequent purification. On the basis, water-soluble impurities are removed through layering under the heating condition, acetonitrile is used for primary crystallization at the low temperature, a crystallization product is diluted with water after being secondarily dissolved with ethyl alcohol, recrystallization is achieved through cooling, and a pure product is obtained after a re