, 1214 (1984).Specific assignment of the non-exchangeable base and ribosc anomcric protons is difficult for oligoribonucleotides with a high pyrimidine content. Problems arise from the narrow range of pyrimidine H-6 chemical shifts and thc ovcrlap of pyrimidine H-5 rcsonanccs with thc ribose anomeric proton signals. To solve thcsc problems two multiple pulsc methods werc used which depend on the scalar coupling betwccn H-6 and H-5. The first method was double-quantum nmr which established the connectivity bctwecn specific pyrimidine H-6 and H-5 rcsonances. A rcfocussing pulse was added to the end of the doublequantum pulse sequence to improve the identification of several H-6 and H-5 connectivities in a single expcriment. The second procedure involved hornonuclcar decouplcd spin ccho nmr to remove H-5 signals sclcctivcly from the ribose anomeric proton region. These techniques are illustrated by the assignment of the spectra of the oligoribonucleotides UpUpC, UpUpU, GpCpUpC, and UpApGpCpUpU.