Shah K, Wu H, Rana T M
Department of Pharmacology, Robert Wood Johnson Medical School, University of Medicine and Dentistry of New Jersey, Piscataway 08854.
Bioconjug Chem. 1994 Nov-Dec;5(6):508-12. doi: 10.1021/bc00030a005.
The synthesis of three new photoactive RNA phosphoramidites, 5-bromouridine, 5-iodouridine, and O4-triazolouridine, is reported. The 5' OH of bromouridine and iodouridine were protected as dimethoxytrityl ether using dimethoxytrityl chloride and pyridine. Selective protection of 2' OH was achieved as the corresponding tert-butyldimethylsilyl ether. Protected ribonucleosides were converted to phosphoramidites using 2-cyanoethyl N,N-diisopropylchlorophosphoramidite. O4-Triazolouridine phosphoramidite monomer was prepared in one step from uridine phosphoramidite. These phosphoramidites were used to incorporate photoprobes at any chosen sites in the RNA sequences during chemical syntheses. The modified monomers were incorporated into RNA oligomers with coupling yields > 98%. After chemical synthesis, O4-triazolouridine was converted to 4-thiouridine by the addition of thiolacetic acid during standard deprotection methods. The extent of thiation and incorporation of modified nucleotides into RNA sequences were confirmed by nuclease digest, HPLC, and gel electrophoresis.
报道了三种新型光活性RNA亚磷酰胺的合成,即5-溴尿苷、5-碘尿苷和O4-三唑尿苷。使用4,4'-二甲氧基三苯甲基氯和吡啶将溴尿苷和碘尿苷的5'-OH保护为二甲氧基三苯甲基醚。通过将相应的叔丁基二甲基甲硅烷基醚实现了2'-OH的选择性保护。使用2-氰基乙基N,N-二异丙基氯亚磷酰胺将受保护的核糖核苷转化为亚磷酰胺。O4-三唑尿苷亚磷酰胺单体由尿苷亚磷酰胺一步制备。在化学合成过程中,这些亚磷酰胺用于在RNA序列中的任何选定位置掺入光探针。修饰的单体以大于98%的偶联产率掺入RNA寡聚物中。化学合成后,在标准脱保护方法中通过加入硫代乙酸将O4-三唑尿苷转化为4-硫尿苷。通过核酸酶消化、HPLC和凝胶电泳确认了硫代程度以及修饰核苷酸掺入RNA序列的情况。