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离子液体[Bmim]BF4既作溶剂又作催化剂合成了螺环磷酰二氯(SPDPC),在原料季戊四醇与三氯氧磷的摩尔比为1∶2.2,反应温度40℃,反应时间7 h的条件下,产率达66%。用熔点、IR和1HNMR表征了SPDPC的结构。推测了离子液体的催化机理。合成方法与文献典型的方法做了比较,结果发现,用离子液体作溶剂和催化剂,不但缩短了反应时间,降低了反应温度,而且不挥发,易回收,经济、环保,是合适的合成SPDPC的溶剂和催化剂。
Spirocyclodichloridate (SPDPC) was synthesized using ionic liquid [Bmim] BF4 as both solvent and catalyst. When the molar ratio of raw material pentaerythritol to phosphorus oxychloride was 1: 2.2, the reaction temperature was 40 ℃ and the reaction time was 7 h Under the conditions, the yield of 66%. The structure of SPDPC was characterized by melting point, IR and 1HNMR. The catalytic mechanism of ionic liquid is presumed. The synthesis method is compared with the typical methods of the literature. The results show that the use of ionic liquid as solvent and catalyst not only shortens the reaction time and reduces the reaction temperature, but also is nonvolatile, easy to recover, economical and environmental friendly and is suitable for synthesizing SPDPC Solvents and catalysts.