The object of the work was to prepare alkoxylated derivatives ofsym-diethyldiphenylurea from methylated and ethylated vanillin. Standard procedures for converting methylated vanillin to 3,4-dimethoxyaniline were extended to the syntheses of the known 3-methoxy-4-ethoxyaniline. The following derivatives of 3,4-dimethoxyaniline are believed to be new: the formanilide, m.p. 91 °C.; sulphonamide, m.p. 132 °C.; N-ethylsulphonamide, m.p. 94 °C.; N-ethylacetanilide, m.p. 62 °C.; and the N-ethylaniline, an uncrystallized oil. Condensations of the last with phosgene yielded the N-ethylcarbamyl chloride, m.p. 86 °C.; N-ethyl-NN'-NN′-(3,4-dimethoxyphenyl)-urea, m.p. 159 °C.; and the correspondingsym-N,N′-diethyl derivative, m.p. 79 °C. N,N′-di-(3,4-dimethoxyphenyl)-urea, m.p. 214 °C., was synthesized by a method that removed previous doubt about its structure. The derivatives of 3-methoxy-4-ethoxyaniline believed to be new are: the hydrochloride, m.p. 221 °C.; the formanilide, m.p. 103 °C.; the N-ethylformanilide, m.p. 80 °C.; and the N-ethylaniline, m.p. 43 °C. Condensations of the last with phosgene gave the N-ethylcarbamyl chloride, m.p. 85 °C.; N-ethyl-N,N′-di-(3-methoxy-4-ethoxyphenyl)-urea, m.p. 127 °C. and the corresponding N,N′-diethyl derivative, m.p. 51 °C. A condensation of 3-methoxy-4-ethoxyaniline with urea resulted in the corresponding monosubstituted urea, m.p. 177 °C.; and N,N′-disubstituted urea, m.p. 209 °C. Yields were uniformly higher than those obtained in the 3,4-dimethoxy series.