NbTi and Nb3Sn superconductors have been synthesized directly from the oxides by electro‐deoxidation, where the cathode is made by placing an intimate mixture of the sintered oxide in a molten bath of calcium chloride and sodium chloride. The favored cathodic reaction is the removal of the oxygen from the oxides to form the superconducting intermetallic alloys and not the deposition of calcium. The superconducting properties of the intermetallic compounds are confirmed.