The synthesis of the superconducting YBa2Cu3O7−xfrom a soluble, molecular precursor with the composition Cu3O3Ba2Y(meOEt)7(meOEt is 2‐methoxyethoxide) is described. The precursor was synthesized from the reaction of a soluble copper (II) oxide polymer with alkoxides of barium and yttrium. Pyrolysis and oxidation of the precursor resulted in the formation of oriented sheets of the orthorhombic YBa2Cu3O7−xphase. The orientation in the bulk YBa2Cu3O7−xis believed to result from the presence of linear Cu‐O‐Cu‐O chains in the precursor. Bulk YBa2Cu3O7−x, prepared from the precursor, had an onset transition temperature of 92.5 K and zero resistance at 89.5 K.