摘要
在浓盐酸存在下，１，４，７，１０－四氮杂环十二烷和１，４，８，１１－四氮杂环十四烷分别与亚磷酸、甲醛发生Ｍａｎｎｉｃｈ型反应，得到相应的Ｎ，Ｎ＇，Ｎ″，Ｎ＇＇＇－四甲膦酸－１，４，７，１０－四氮杂环十二烷（ＤＯＴＰ）和Ｎ，Ｎ＇，Ｎ″，Ｎ＇＇＇－四甲膦酸－１，４，８，１１－四氮杂环十四烷（ＴＥＴＰ），产物纯度较高。在不同的ＰＨ值条件下测定了产物的１ＨＮＭＲ，考察了其化学位移的变化。在此基础上，采用改进的大环配体络合物直接合成法，合成了ＤＯＴＰ和ＴＥＴＰ的Ｌａ３＋、Ｇｄ３＋络合物。
Tetraazacyclodecane-N, N', N', N'''-tetramethylenephosphonic acid (DOTP) and 1,4,8,11-tebraazacyclotetradecane-N, N', N',N'''-tetramethylenephosphonic acid (TETP) were respectively synthesized by Mannich-type reactions of 1, 4,7,10-tetraazacyclododecane and 1, 4, 8, 11-tetraazacyclotetradecanewith phosphorous acid and formaldehyde in thepresence of concentrated hydrochloric acid. The PH dependence of the chemical shifts of the peaks exhibitedby these macrocyclic aminophosphonic acids was studied. And then,La3+ and Gd3+ complexes with DOTP orTETP were prepared with an improved synthetic technique of macrocyclic compounds.
出处
《化学试剂》
CAS
CSCD
北大核心
1996年第2期73-75,共3页
Chemical Reagents
关键词
四氮杂环
氨基膦酸
镧
钆
配合物
tetraazacyclododecane, 1, 4, 8, 11- tetraazacyclotetradecane, 1, 4, 7, 10-tetraazacyclodode cane-N, N', N', N'''-tetramethylenephosphonic acid, 1,4, 8, 11-tetraazacyclotetradecane-N, N', N', N'''-tetramethylenephosphonic acid, La3+ complexes, Gd3+ complex
