The article describes the features of the synthesis of a new oxide pyrochlore Bi2.7Ni0.7Mg0.46Sb2O10+? (sp. gr. Fd-3m, a = 10.4703 ?) containing antimony (V) and bismuth (III) cations from a stoichiometric mixture of oxide precursors using a modified sol-gel method (method Pecini). It is shown that the formation of antimony (III, V) and bismuth (III) compounds that are volatile upon calcination can be prevented by dissolving the precursors in sulfuric or nitric acid solutions, and excluding the use of hydrochloric acid or chloride solutions. A step-by-step synthesis of two samples obtained from sulfuric and nitric acid media was carried out, and the phase composition of the preparations calcined in the temperature range of 350…950 ?C was analyzed. When calcining the sample obtained from the sulfuric acid solution, the Bi12.67O14(SO4)5 phase was revealed, which prevents the formation of pyrochlore in the low-temperature region. In the sample synthesized from the nitric acid solution, bismuth stibates Bi3SbO7, BiNbO4 are recorded as intermediate phases Sb2O4, Bi12MgO19, Bi7.47Ni0.53O11.73, Bi3Ni2/3Sb5/3O11, NiSb2O6 were identified as other intermediate phases in the samples. The synthesis temperature of single-phase Bi2.7Ni0.7Mg0.46Sb2O10+? with the pyrochlore structure is 950 ?С. The phase purity and chemical composition of the sample were established by X-ray phase analysis and energy-dispersive X-ray analysis.