The disclosure herein pertains to herbicidal methods and compositions containing 3,5-dicarboxylic acid esters of 2,6-bis-(fluoroalkyl) tetrahydropyrans and piperidines which may be substituted in the 4-position by certain alkyl, phenyalkyl, phenyl, alkoxyalkyl, alkylthioalkyl, cycloalkyl, and heterocyclic radicals wherein the hetero atom is oxygen and sulfur and to a process for the preparation thereof. These compounds are useful as pre-emergent herbicides.