摘要
以环戊二烯二聚体、顺丁烯二酸酐、溴、乙二胺为主要原料，经五步反应合成了Ｎ，Ｎ′１，２乙烷双［５，６二溴降冰片烷２，３二酰亚胺］（Ⅰ）。其中前四步反应与文献［１］相同，第五步反应，取２２５ｇＮ，Ｎ′１，２乙烷双［５，６二溴３羧基降冰片烷２酰胺］（Ⅱ）于三口烧瓶中，加入８５ｍｌ二甲苯、３２ｍｌ丙酸、４滴磷酸，加热、搅拌回流脱水５ｈ，冷却、过滤，依次用甲苯—丙酸混合液和２％ＮａＯＨ水溶液洗涤，干燥，得１９８ｇ白４２色固体，产率８５％，与文献［１］相当。新的合成方法操作条件好，产品色泽好，成本低。提出了第五步反应可能的机理。
The title compound(Ⅰ) is synthesized in 5 steps with dicyclopentadiene,maleic anhydride,bromine and ethylenediamine as main raw materials.In the fifth step reaction,85ml xylene and 32ml propionic acid and 4 drops of H 3PO 4 are added to 22.5g N,N′ 1,2 ethane bis[5,6 dibromo 3 carboxy norbornane 2 amide](Ⅱ).The mixture is stirred and refluxed to dehydrate for 5h,cooled and filtered,washed by the mixture of toluene and propionic acid and 2% NaOH aq.respectively,dried and got 19.8g Ⅰ which is white solid.The yield is 85%. The new method is easier to control,and cost is lower.The possible mechanism of the fifth step reaction is presented .
出处
《精细化工》
EI
CAS
CSCD
北大核心
1998年第3期41-44,共4页
Fine Chemicals
关键词
阻燃剂
聚烯烃
二溴降冰片烷
二酰亚胺
fire retardant,polyolefine,N,N′ 1,2 ethane bis[5,6 dibromonorbornane 2,3 dicarboximide]
