This paper aims to optimize the liquid repellency performance of fluorochemical urethane (FU)—a patented technology with a shorter fluorocarbon chain (C4). FU is free from persistent bioaccumulative toxins such as perfluorooctanoic acid (PFOA) and perfluorooctanesulfonate (PFOS), unlike the long-chain fluorinated chemicals (>C6). Different sets of varied finish concentrations with an extender and a wetting agent were prepared to treat the 65/35% polyester/cotton blended fabric. The finish concentration was optimized based on the liquid repellency (water and oil-repellency) of the treated fabric and its laundering durability. In addition, the effect of the finish concentration on selected physical properties of the treated fabric was studied as well. The liquid repellency, laundering durability, and selected physical properties of the treated and untreated fabrics were analyzed using ASTM and AATCC standard test methods. The results of textile substrates treated with 60 g/L of FU show an optimum balance of desired liquid repellency without affecting the physical properties of the fabric significantly.