An efficient and eco-friendly procedure has been developed for the synthesis of various 2,2'arylmethylenebis(3-hydroxy-5,5-dimethyl-2-cyclohexene-1-one) derivatives which were isolated and characterized by melting point, IR, 1 H-NMR, 13 C-NMR and mass spectrometric techniques. Out of the fourteen compounds synthesized, four compounds yielded crystals suitable for single crystal X-ray analysis which showed that 2,2'-phenylmethylenebis(3-hydroxy-5,5-dimethyl-2-cyclohexene-1-one) crystallizes in the tetragonal system with space group I 4 1 /a, 2,2'-(3-nitrophenyl)methylenebis(3-hydroxy-5,5-dimethyl-2-cyclohexene-1-one) crystallizes in the monoclinic system with space group P 2 1 /n, 2,2'-(4-nitrophenyl)methylenebis(3hydroxy-5,5-dimethyl-2-cyclohexene-1-one) crystallizes in the orthorhombic system with space group Pca21 and 2,2'-(4-chlorophenyl)methylenebis(3-hydroxy-5,5-dimethyl-2-cyclohexene-1-one) crystallizes in the monoclinic space group P21/c.
An eco-friendly and expedient procedure for one-pot synthesis of bis-(indolyl)methane derivatives via electrophilic substitution reaction at C-3 position of indole with various aldehydes has been developed by using silica-diphenic acid as a novel heterogeneous catalyst. This method has various promising features such as short reaction time, easy work-up procedure, good yield of products and remarkable activity and selectivity of the catalyst.
Sulfoacetate modified silica supported Indium(III) triflate [SiSAIn (OTf) 2 ], a novel solid acid catalyst was synthesized and characterized by various spectroscopic techniques such as TEM, SAED, SEM, TGA and FTIR. The synthesized catalyst has proved its catalytic potential for the synthesis of 1,2,4,5-tetrasubstituted imidazole derivatives by the reaction among various substituted aromatic aldehydes, benzil, substituted aromatic amines and ammonium acetate. The synthesized derivatives were characterized by IR, 1 H-NMR, 13 C-NMR and mass spectroscopy. Among the various synthesized derivatives, 1,2,4,5-tetraphenyl-1H-imidazole (C 27 H 20 N 2 ) derivative was grown into good crystalline form and crystallizes in the triclinic space group P-1 with the unit-cell parameters: a = 9.9395(7), b = 10.0204(8), c = 20.8332(16) Å, α = 80.791 (7), β = 82.138(6), γ = 82.878(7)°and Z = 4. The crystal structure was solved by direct methods using single-crystal X-ray diffraction data collected at room-temperature and refined by full-matrix least-squares procedures to a final R-value of 0.0516 for 3111 observed reflections.Analysis of TEM micrographs of the catalyst sulfoacetate modified silica supported indium triflate [SiSAIn(OTf) 2 ] revealed the particle size and morphology of above synthesized [a] R.
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