Titanium aluminide is synthesized in a chemical reaction of elemental powders. The synthesis is conducted at a high temperature in vacuum for two variants of pressure variation. To obtain a quality product at a minimum loss of the material to spillage, it is important to apply pressure at the right moment. The reaction synthesis is also accompanied by “swelling” of the billet. The temperature-pressure cycle is optimized. The results of the x-ray diffractometry show the presence of an aluminum-rich phase in the form of a shell surrounding the particles of pure titanium.