The study revealed peculiarities in the formation of mixed oxides with the Mn3-xAlxO4 spinel structure that were obtained from initial simple oxides beta-Mn3O4 and gamma-Al2O3 by calcination in various media at 600-1200 degrees C. The phase composition of the samples treated in air, argon or hydrogen was investigated using ex situ and in situ X-ray diffraction. It was shown that the occurrence of phase transformations depends on the treatment conditions and is related to the charge state of manganese cations. A scheme of the structural transformations induced by temperature and medium was proposed. The formation temperature of spinel was found to decreases from 950 to 600 degrees C when the oxidizing medium is replaced by the reducing one. Mn3-xAlxO4 spinel (x similar to 1.5) was produced in air at temperatures above 1050 degrees C or in an inert medium at 800-1200 degrees C.