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Ultra-high-purity propylene glycol monomethyl ether acetate (PGMEA) is required as a solvent to meet the stringent requirements of the electronic-grade semiconductor industry. Here, a comparative study of two process intensification configurationsa coupling reaction and separation in the transesterification route for PGMEA productionis presented. Reactive distillation (RD), despite being technically feasible for the transesterification reaction, poses severe challenges owing to its operational/design limitations. For instance, the homogeneous catalyst sodium methoxide is insoluble in the reaction mixture and deposited on the reactive packing surface of the RD column. An intensified configuration of the side-reactor column (SRC) configuration is analyzed as an alternative to mitigate the operational limitations of RD. An economic evaluation is conducted for both configurations, showing that the SRC configuration can match the performance of an RD column with only a 5% increase in total annual cost.