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A Lewis acid- and base-co-mediated cyclization of trifluoroacetyl diazoester and ketones is developed. Cooperative functioning of the Lewis acid and Lewis base with trifluoroacetyl diazoester results in increased electrophilicity of terminal nitrogen atoms. The reaction affords polysubstituted 4-trifluoromethyl pyrazoles in moderate to excellent yields.Cytometry of Reaction Rate Constant (CRRC) uses time-lapse fluorescence microscopy to measure a rate constant of a catalytic reaction in individual cells and, thus, facilitate accurate siz