Quadratic criterion-based iterative learning control (QILC) was applied to a numerical reactive batch distillation process, in which methacrylic anhydride (MAN) is produced through the reaction of methacrylic acid with acetic anhydride. The role of distillation is to shift the equilibrium conversion toward the direction of the product by removing acetic acid (AcH), a by-product of the reaction. Two temperatures at both ends of the column were controlled by individual control loops. A nonlinear PID controller manipulating the reflux ratio was employed to regulate the top temperature at the boiling point of AcH. A constrained QILC was used for the tracking of the reactor temperature. A time-varying reference trajectory for the reactor temperature that satisfies the target conversion and purity of MAN was obtained through repeated simulations and confrimation experiments in the pilot plant. The QILC achieved satisfactory tracking in several batch runs with gentle control movements, while the PID control as a substitute of the QILC in a comparative study exhibited unacceptable performance.