The synthesis of methyl fluoroacetate consists of a two-step process:
# Potassium fluoride (KF) and the catalyst are added into the solvent within the reactor; this is then stirred and heated up. The catalyst mentioned in this step is a phase-transfer catalyst and can be the chemicals dodecyl(trimethyl)ammonium chloride , tetrabutylammonium chloride , tetrabutylammonium bromide , or tetramethylammonium chloride . The mass ratio of the potassium fluoride and the catalyst in this step is 0.5~1 : 0.02~0.03. With the solvent mentioned in this step being a mixture of dimethylformamide () and acetamide () with a mass ratio of 1.4~1.6: 1. The mass ratio of the solvent and potassium fluoride is 1.1~2.0 : 0.5~1.
# When the reaction temperature of 100~160 °C is reached, methyl chloroacetate  is continuously added in the reactor at a speed of 5~10 kg/min with the mass ratio of methyl chloroacetate and potassium fluoride being 1:0.5～1. The reaction between these chemicals produces a gas mixture, with the gases within this mixture then being split between two condensers according to their condensation temperature. Methyl chloroacetate is condensed within the condenser set at 100~105 °C, it is then returned to the reactor to continue participating in the chemical reaction. Methyl fluoroacetate in the other condenser then enters a two-stage nitration condensation at a temperature of 20~25 °C which then ensures that the methyl fluoroacetate is condensed into a liquid with it being the product of this reaction.