The relationship between NMR chemical shifts of adenine ring protons of low concentrations of 9, 9′-(alkane-α, ω-diyl) diadenine and the length of the polymethylene chains has been investigated in buffer solutions at pD 1.0, 7.0 and 13.0 and in organic solvents such as CD3OD,(CF3) 2CDOD,[2H6] dimethyl sulfoxide and CF3COOD. The chemical shifts were compared with those of 9-(ω-bromoalkyl) adenine.