The organomercury compounds HgR2 (R = 2‐Cl,6‐FC6H3, 2,6‐F2C6H3, 2,3,6‐F3C6H2, m‐HC6F4, p‐HC6F4, or C6F5) and RHg(O2CR) (R = 2‐Cl,6‐C6H3, 2,6‐F2C6H3 or 2,3,6‐F3C6H2) have been obtained in moderate – good and low yields respectively from decarboxylation reactions of the corresponding mercury(II) fluorobenzoates in boiling pyridine. By contrast, mercury(II) 2,3,4‐5‐tetrafluorobenzoate gave a low yield of CO2, a trace of Hg(o‐HC6F4)2 and a very low yield of o‐HC6F4Hg(O2CC6F4H‐o). The 199Hg NMR spectra of the diorganomercurials (R = 2‐Cl,6‐FC6H3, 2,6‐F2C6H3, 2,3,6‐F3C6H2, 2,4,6‐F3C6H2, 2,6‐Cl2C6H3, o‐HC6F4, m‐HC6F4, p‐HC6F4 or C6F5) are discussed.