Linear diribonucleoside phosphotriester is an important intermediate for synthesizing biologically important compounds,such as cyclic bis(3’-5’) diguanylic acid(c-di-GMP) and its analogues. Atropisomerism of diastereomers generated by the chiral center of the P atom,which results in the doubling of signals in ~(31)P NMR.The data of ~(31)P NMR at different temperature are presented,and thereafter the reason is discussed. Linear diribonucleoside phosphotriester is an important intermediate for synthesizing biologically important compounds such as cyclic bis (3’-5 ’) diguanylic acid (c-di-GMP) and its analogues. Atropisomerism of diastereomers generated by the chiral center of the P atom, which results in the doubling of signals in ~ (31) P NMR. The data of ~ (31) P NMR at different temperature are presented, and thereafter the reason is discussed.