化学研究与应用
化學研究與應用
화학연구여응용
CHEMICAL RESEARCH AND APPLICATION
2014年
1期
140-144
,共5页
2-(4-异硫氰基苄基)-1,4,7,10-四氮杂环十二烷四乙酸%偶联剂%放射免疫治疗
2-(4-異硫氰基芐基)-1,4,7,10-四氮雜環十二烷四乙痠%偶聯劑%放射免疫治療
2-(4-이류청기변기)-1,4,7,10-사담잡배십이완사을산%우련제%방사면역치료
p-SCN-Bz-DOTA%bifunctional chelator%radioimmunotherapy
以对硝基苯丙氨酸和乙二胺为原料,经酯化、胺解、成环、烷基化、还原、取代等反应合成了目标产物2-(4-异硫氰基苄基)-1,4,7,10-四氮杂环十二烷四乙酸(p-SCN-Bz-DOTA),总产率为10．4%。反应中使用NaBH4/BF3体系代替甲硼烷作为还原剂,提高了操作过程的安全性；使用溴乙酸叔丁酯代替溴乙酸作为烷基化试剂,提高了烷基化的反应产率,而且避免了使用制备型高效液相色谱,降低了合成成本。
以對硝基苯丙氨痠和乙二胺為原料,經酯化、胺解、成環、烷基化、還原、取代等反應閤成瞭目標產物2-(4-異硫氰基芐基)-1,4,7,10-四氮雜環十二烷四乙痠(p-SCN-Bz-DOTA),總產率為10．4%。反應中使用NaBH4/BF3體繫代替甲硼烷作為還原劑,提高瞭操作過程的安全性；使用溴乙痠叔丁酯代替溴乙痠作為烷基化試劑,提高瞭烷基化的反應產率,而且避免瞭使用製備型高效液相色譜,降低瞭閤成成本。
이대초기분병안산화을이알위원료,경지화、알해、성배、완기화、환원、취대등반응합성료목표산물2-(4-이류청기변기)-1,4,7,10-사담잡배십이완사을산(p-SCN-Bz-DOTA),총산솔위10．4%。반응중사용NaBH4/BF3체계대체갑붕완작위환원제,제고료조작과정적안전성；사용추을산숙정지대체추을산작위완기화시제,제고료완기화적반응산솔,이차피면료사용제비형고효액상색보,강저료합성성본。
Target product p-SCN-Bz-DOTA was synthesized using p-nitrophenylalanine and ethylenediamine as the starting materials through esterification, amine solution, cyclization, alkylation, reduction and substitution reactions, with a total yield of 10. 4%. NaBH4/BF3 was used as the reductant instead of borane,and the safety of operation process was improved. By using of tert-butyl es-ter bromoacetate as the alkylating agent instead of bromic acid,the yield of alkylation was increased,and a preparative high perform-ance liquid chromatography was unnecessary for the purification,which could lead to decrease of the cost.
