In this paper, a rapid, easy and very efficient method for the synthesis of bis(pyrazolyl)methanes has been reported in the presence of nickel–guanidine complex immobilized on MCM-41 (MCM-41@Gu@Ni) as a recyclable nanocatalyst. This mesoporous silica catalyst was effective for the one-pot multi-component reaction of arylaldehydes, phenylhydrazine and ethyl acetoacetate in ethanol solvent. The current synthesis shows attractive features, for example the use of recoverable and reusable nanocatalyst (5 times), easy workup, suitable one-pot procedure, short reaction times, good to excellent yields and moderate reaction conditions.