节点文献
1,4-二(5,5-二甲基-1,3-二氧杂己内磷酰亚胺基)苯的合成
Synthesis of 1,4 Bis(5,5 dimethyl 1,3 dioxacyclophosphorimide)benzene
【摘要】 对以新戊二醇、三氯氧磷和对苯二胺为原料,在三乙胺和4N,N二甲胺基吡啶(DMAP)催化作用下合成1,4二(5,5二甲基1,3二氧杂己内磷酰亚胺基)苯(NBPAN)的反应进行了研究。讨论了DMAP对该反应的作用机制,合成收率达82.7%。并用元素分析、IR和1HNMR表征了产物的结构。热重分析表明NBPAN的起始分解温度为280℃,并在280~310℃迅速炭化,成炭率达35.58%。
【Abstract】 Bis(5,5 dimethyl 1,3 dioxacyclophosphorimide)benzene is synthesized by the intermedia of phosphorylation reaction of neopentyl alcohol and POCl 3,and p phenyldiamine in the presence of Et 3N and 4 N,N methylaminopyridine.The total synthetic yield is about 82.7%.The outstanding catalysis of DMAP is studied . The structure of NBPAN is confirmed by elementary analysis ,IR and 1 HNMR.The result of thermogravimetry shows that the beginning temperature of NBPAN decomposition is above 280℃,and rapidly carbonized between 280℃ and 310℃.The char yield is about 35.58% at 500℃.
【Key words】 cyclic phosphate; phosphorimide; phosphorylation; intumescent flame retardant;
- 【文献出处】 精细化工 ,FINE CHEMICALS , 编辑部邮箱 ,1999年01期
- 【分类号】TQ569,TQ265.1
- 【被引频次】40
- 【下载频次】242