Nesmeyanov, together with N.K. Kochetkov and M.I. Rybinskaya, developed a method for the synthesis of various five- and six-membered heterocycles, which is based on the high activity of carbonyl groups and the mobility of the β-substituent in compounds of the type RCOCH=CHX. The same group of scientists developed the method of "β-ketovinylation", which consists in introducing an RCOCH=CH group into the molecule. The reaction of β-substituted vinyl ketones with an azide ion made it possible to study the stereochemistry and propose a mechanism for nucleophilic substitution at the activated double bond.
In collaboration with other scientists, Nesmeyanov carried out a number of works in the field of radical telomerization and rearrangement radicals. In addition to studies of already known reactions, thermal telomerization of ethylene and propylene with silicon hydrides has been developed and other new telomerization reactions. Also, new routes for the synthesis of compounds containing groups such as CCl, CClCHCl, CClC=CH, CCl=CHX and others. The study of compounds containing the CCl-C=CCBr=CH to CCl=CClCHBr under ultraviolet illumination.
In continuation of the work related to the previously created diazo method, Nesmeyanov and L. G. Makarova investigated the mechanism of decomposition of aryldiazonium and diaryliodonium salts. This made it possible to synthesize new types of onium compounds - diphenylbromonium, diphenylchloronium and triphenyloxonium salts. Together with T. P. Tolstaya and other scientists, Nesmeyanov showed that double salts of diphenylbromonium and diphenylchloronium halides with heavy metal halides are decomposed by powders of the corresponding metals with the formation of organometallic compounds. Thus, the diazo method began to be used to obtain σ-aryl complexes of transition metals and other organometallic compounds.