We report on chemical polymerization of two aniline derivatives - 2-methylaniline and 2-methoxyaniline -- in a two-phase water/pentane system. We have found that poly(2-methylaniline) is produced in form of an amorphous material regardless of the fact whether the monomer is initially dissolved in aqueous or organic phase. The behavior of 2-methoxyaniline is significantly different. The oxidation of this monomer generally results in formation of a water soluble oligomer and an insoluble polymeric product. In consequence, depending on the experimental setup, the polymer is prepared in form of a thin film at the organic/aqueous interface or as micrometer-sized spherical particles dispersed in the aqueous phase.