V. F. Makarov

Inclusion compounds ofcis-syn-cis andcis-anti-cis diastereoisomers of dicyclohexano-18-crown-6 with amidosulfuric acid

Both title complexes were prepared by reacting a methanol solution of the respective isomer of dicyclohexano-18-crown-6 (DCH18C6) with an aqueous solution of amidosulfuric acid. Crystals suitable for X-ray crystallography were obtained by recrystallization from methanol.Crystals of [cis-syn-cis-DCH18C6][NH2SO2OH·CH3OH] (1) are monoclinic, space groupP21ln,a = 21.700(8),b = 13.725(5),c = 9.118(6) Å,ψ = 76.29(2) Å. Refinement led to a final conventionalR value of 0.065 for 2083 reflections. [Cis-anti -cis-DCH18C6][NH2SO2OH] (2) crystallizes in the orthorombic space groupPna21 with unit cell dimensionsa = 17.154(7),b = 16.051(7),c =8.630(5) Å. Refinement was terminated at anR value of 0.067 for 1936 reflections.

1,2-DIISOPHTHALIMIDOETHANE. X-RAY DIFFRACTION EVIDENCE FOR THE STRUCTURE OF THE PRODUCT OF ACYLATION OF 1,2-DIAMINOETHANE WITH PHTHALOYL CHLORIDE

It was demonstrated by x-ray diffraction investigation of the product of the reaction of 1,2-diaminoethane with phthalic acid dichloride that the resulting compound has the 1,2-diisophthalimidoethane structure. An improved method for its synthesis is proposed.

Acylation of aza crown ethers with N-substituted isophthalimides

Acylated aza crown ethers containing fragments of N-substituted phthalamic acids in the side chain were obtained by the reaction of monoaza-15-crown-5, monoaza-18-crown-6, and diaza-18-crown-6 with N-substituted isophthalimides.

Structure of 1,4,7,10,13-pentaoxa-16-(sulfanil)azacyclooctadecane

The crystal structure of 1,4,7,10,13-pentaoxa-16-(sulfanil)azacyclooctadecane was determined in an x-ray diffraction structural analysis. This structure consists of centrosymmetric hydrogen-bonded dimers of independent 1,4,7,10,13-pentaoxo-16-(sulfanil)azacyclooctadecane molecules and is a host-guest autocomplex, in which the macrocyclic part of the molecule is the host and the sulfanil substituent of another molecule is the guest.

Synthesis and structures of molecular complexes of the cis-anti-cis diastereomer of dicyclohexano-18-crown-6 with o-nitroanilines

In the reaction of the cis-syn-cis and cis-anti-cis diastereomers of dicyclohexano-18-crown-6 with 2-nitro and 2,4-dinitroaniline crystalline complexes with a 1:2 stoichiometric composition were obtained only when the cis-anti-cis diastereomer was used. The three-dimensional structure of the complex of the cis-anti-cis diastereomer of dicyclohexano-18-crown-6 with 2,4-dinitroaniline was determined by an x-ray diffraction study. The complexing of o-nitroanilines with the cis-anti-cis diastereomer is explained by the topological conformity of the interacting compounds. The isolation of the individual cis diastereomers from the mixture of them formed as a result of the catalytic hydrogenation of dibenzo-18-crown-6 was accomplished by means of the selective formation of the crystalline complex of the cis-anti-cis diastereomer with 2-nitroaniline.

Crown ethers bound to sulfanilamide preparations

Complexes with a 1∶2 composition were obtained by the reaction of 8-crown-6 ethers with 4-aminobenzenesulfonamide and 4-aminobenzensulfoguanidine. Crown ethers containing a sulfanilyl group were obtained in the reaction of azacrown ethers with 4-acetylaminobenzenesulfonyl chloride.