<p>Monochloroacetaldehyde alkoxycarbonylhydrazones of the formula Cl-CH2-CH=N-NH-COOR in which R is an alkyl group are produced in a high purity and in a high yield by decomposing monochloroacetaldehyde trimer into monochloroacetaldehyde monomer and then reacting the monomer with an alkyl carbazate H2N-NH-COOR in an organic solvent.</p>