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Amorphous mesoporous materials are promising as catalysts for processes involving or forming bulk molecules. In a reaction such as acetone condensation to form mesitylene, an effective catalyst should not only have a developed porous structure but also have active centers of acidic and basic types. The sol–gel approach allows one to obtain titanosilicates with such characteristics. This work demonstrates the possibility of controlling their properties by varying the conditions for the synthesis of titanosilicate gels. It has been established that controlling hydrolysis allows one to increase the activity of amorphous mesoporous titanosilicates by 10 times: from acetone conversion of 6% to 60%. It has been shown that the use of titanium acetylacetonate complexes in the synthesis of gels leads to an increase in the content of tetracoordinated Ti in the structure and contributes to an increase in the acidity of titanosilicates. During the condensation of acetone on the obtained mesoporous titanosilicates, high acetone conversion (60–79%) and mesitylene selectivity of up to 83% were achieved. [ABSTRACT FROM AUTHOR]