The reaction between p-nitrobenzyl 2-diazoacetoacetate and trimethylchlorosilane (TMS-Cl) produces a toluene-soluble silylenol ether (SEE) product and insoluble byproduct salts (NaCl and triethylammonium hydroiodide). Purification of the SEE solution via removal of the salts and unreacted TMS-Cl is accomplished by integrating two unit operations [crossflow microfiltration and distillation in a wiped-film evaporator (WFE)] into a semicontinuous process. The process addresses the critical scale-up issues of potential exothermic activity near the operating temperature, water sensitivity of the product, and the avoidance of direct solids handling. Key to its successful scaleup from the laboratory (2 kg scale) to manufacturing (370 kg scale) was the development of a distributed control system which addresses characteristics unique to each of the unit operations. Crossflow operation at all scales exhibited a substantial increase and then a decrease in transmembrane pressure (TMP) which coincided with dissolved solids concentration and concomitant solution viscosity. Membrane fouling, which became apparent in manufacturing after repeated membrane use, was addressed by operational changes to minimize TMP and by incorporating a membrane cleaning procedure.