摘要
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。
SPDPC was synthesized in Ion Liquid [ Bmim ] BF4 as solvent and catalyst. Pentaerythritol reacted with phosphorus oxychloride in 1：2. 2 molar ratio at 40 ~C for 7 h with a yield of 66%. The structure of SPDPC was characterized by means of MP, IR and 1HNMR. The catalytic mechanism of Ion Liquid was speculated. The new way was compared with the traditional ones. It is found that Ion Liquid as solvent and catalyst not only shortened the time of reaction and reduced the reactive temperature, but avoided volatilizing, indicating its merits of being more collectable, economical and environmental friendly as a suitable solvent and catalyst for SPDPC synthesis.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2014年第5期676-680,共5页
Fine Chemicals
