Biologically active Bis(indolyl)methanes have been synthesized by using NiSO4.6H2O as a catalyst in C2H5OH at room temperature. NiSO4.6H2O in C2H5OH was found to be an efficient, moisture tolerant and reusable catalyst in reaction of indole with different carbonyl compounds giving corresponding derivatives of Bis(indolyl)methanes. The attractive features of this protocol involve mild reaction condition, excellent yields, simple work up procedure and recyclability of catalyst.