Stein A, Iversen P L, Subasinghe C, Cohen J S, Stec W J, Zon G
Medicine Branch, National Cancer Institute, Bethesda, Maryland 20892.
Anal Biochem. 1990 Jul;188(1):11-6. doi: 10.1016/0003-2697(90)90521-a.
The title compounds were chemically synthesized as their 5'-dimethoxytrityl derivatives by base-catalyzed reaction of 35S-enriched elemental sulfur with support-bound hydrogen phosphonate oligomer. This was derived from adamantane carbonyl chloride-activated coupling of nucleotide hydrogen phosphonate monomers, and similarly activated capping with isopropyl phosphite. A convenient, disposable, reversed-phase cartridge was utilized to purify and isolate the 5'-dimethoxytrityl derivative for subsequent in situ detritylation and elution of the final product. The specific activity obtained for the title compounds was ca. 10(7) cpm/mumols-eq P(O)S-. The procedure should be readily adaptable to appropriate syntheses of other P-S containing analogs of DNA and RNA.
通过将富含35S的元素硫与载体结合的氢膦酸酯低聚物进行碱催化反应，将标题化合物化学合成为其5'-二甲氧基三苯甲基衍生物。这是由金刚烷羰基氯活化的核苷酸氢膦酸酯单体偶联反应得到的，并用亚磷酸异丙酯进行类似活化封端反应得到的。使用一种方便的一次性反相柱来纯化和分离5'-二甲氧基三苯甲基衍生物，以便随后对最终产物进行原位脱三苯甲基化和洗脱。标题化合物获得的比活约为10(7) cpm/μmol-eq P(O)S-。该方法应易于适用于其他含P-S的DNA和RNA类似物的适当合成。
