Scaringe S A, Francklyn C, Usman N
Department of Biology, Massachusetts Institute of Technology, Cambridge 02139.
Nucleic Acids Res. 1990 Sep 25;18(18):5433-41. doi: 10.1093/nar/18.18.5433.
The preparation of fully protected diisopropylamino-beta-cyanoethyl ribonucleoside phosphoramidites with regioisomeric purity greater than 99.95% is described. It is demonstrated that the combination of standard DNA protecting groups, 5'-O-DMT, N-Bz (Ade and Cyt), N-iBu (Gua), beta-cyanoethyl for phosphate, in conjunction with TBDMS for 2'-hydroxyl protection, constitutes a reliable method for the preparation of fully active RNA. Average stepwise coupling yields in excess of 99% were achieved with these synthons on standard DNA synthesizers. Two steps completely deprotect the oligoribonucleotide and workup is reduced to a fifteen minute procedure. Further, it is shown that the deprotected oligoribonucleotides are free from 5'-2' linkages. This methodology was applied to the chemical synthesis of a 24-mer microhelix, a 35-mer minihelix and two halves of a catalytic 'Hammerhead Ribozyme'. These oligoribonucleotides were directly compared in two distinct biochemical assays with enzymatically (T7 RNA polymerase) prepared oligoribonucleotides and shown to possess equal or better activity.
描述了制备区域异构体纯度大于99.95%的完全保护的二异丙基氨基-β-氰基乙基核糖核苷亚磷酰胺的方法。结果表明,标准DNA保护基团(5'-O-DMT、N-Bz(腺嘌呤和胞嘧啶)、N-iBu(鸟嘌呤))、用于磷酸酯的β-氰基乙基以及用于2'-羟基保护的叔丁基二甲基硅烷基(TBDMS)的组合,构成了制备完全活性RNA的可靠方法。使用这些合成子在标准DNA合成仪上实现了平均逐步偶联产率超过99%。两步即可完全脱保护寡核糖核苷酸,后处理简化为15分钟的操作流程。此外,结果表明脱保护的寡核糖核苷酸不存在5'-2'连接。该方法应用于化学合成24聚体微螺旋、35聚体小螺旋以及催化性“锤头状核酶”的两个半体。将这些寡核糖核苷酸在两种不同的生化测定中与酶促(T7 RNA聚合酶)制备的寡核糖核苷酸直接比较,结果显示它们具有同等或更好的活性。