Six novel thiosemicarbazones containing sugar and thiosemicarbazide moieties were synthesized by a five-step procedure using D-galactose and D-xylose as the starting materials and the corresponding glycosyl isothiocyanates as the intermediates. The target compounds were characterized by IR, ^1H NMR, and elemental analysis. The coupliug constants between H1 and H2 in the sugar rings, all fail within the range of J = 9. 2-10.0 Hz, confirming the β-configuration of the compounds.
A new complex of N,N?-bis(p-nitrophenyl)-2,2?-(p-phenylene-dioxy) diacetamide DMF monohydrate, C25H25N5O9·H2O (Mr = 557.52), has been synthesized and its structure was determined by X-ray crystallography method. The crystal belongs to monoclinic system, space group P21/c with a = 7.2812, b = 25.5894, c = 14.3434 ?, β = 91.110(1)o, V = 2672.0(2) ?3, Dc = 1.386 g/cm3, F(000) = 1168, μ = 0.109 mm-1 and Z = 4. The final R = 0.0493 and wR = 0.1173 for 3389 observed reflections with I > 2σ(I). The asymmetric unit of the title complex consists of monomeric N,N?-bis(p-nitrophenyl)-2,2?-(p-phenyleneioxy)diacetamide 1, one DMF and one water molecule, which are incorporated during recrystallization. The molecules are linked into a three-dimensional network by π…π interactions as well as intermolecular interactions among DMF, water molecule and 1.
