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1.
Vinutha V. Salian Badiadka Narayana Hemmige S. Yathirajan Mehmet Akkurt
mer elik Cem Cüneyt Ersanl Christopher Glidewell 《Acta Crystallographica. Section C, Structural Chemistry》2015,71(7):610-617
Four compounds are reported, all of which lie along a versatile reaction pathway which leads from simple carbonyl compounds to terphenyls. (2E)‐1‐(2,4‐Dichlorophenyl)‐3‐ [4‐(prop‐1‐en‐2‐yl)phenyl]prop‐2‐en‐1‐one, C18H14Cl2O, (I), prepared from 4‐(prop‐1‐en‐2‐yl)benzaldehyde and 2,4‐dichloroacetophenone, exhibits disorder over two sets of atomic sites having occupancies of 0.664 (6) and 0.336 (6). The related chalcone (2E)‐3‐(4‐chlorophenyl)‐1‐(4‐fluorophenyl)prop‐2‐en‐1‐one reacts with acetone to produce (5RS)‐3‐(4‐chlorophenyl)‐5‐[4‐(propan‐2‐yl)phenyl]cyclohex‐2‐en‐1‐one, C21H21ClO, (II), which exhibits enantiomeric disorder with occupancies at the reference site of 0.662 (4) and 0.338 (4) for the (5R) and (5S) forms; the same chalcone reacts with methyl 3‐oxobutanoate to give methyl (1RS,6SR)‐4‐(4‐chlorophenyl)‐6‐[4‐(propan‐2‐yl)phenyl]‐2‐oxocyclohex‐3‐ene‐1‐carboxylate, C23H23ClO3, (III), where the reference site contains both (1R,6S) and (1S,6R) forms with occupancies of 0.923 (3) and 0.077 (3), respectively. Oxidation, using 2,3‐dichloro‐5,6‐dicyano‐1,4‐benzoquinone, of ethyl (1RS,6SR)‐6‐(4‐bromophenyl)‐4‐(4‐fluorophenyl)‐2‐oxocyclohex‐3‐ene‐1‐carboxylate, prepared in a similar manner to (II) and (III), produces ethyl 4′′‐bromo‐4‐fluoro‐5′‐hydroxy‐1,1′:3′,1′′‐terphenyl‐4′‐carboxylate, C21H16BrFO3, (IV), which crystallizes with Z′ = 2 in the space group P. There are no significant intermolecular interactions in the structures of compounds (I) and (II), but for the major disorder component of compound (III), the molecules are linked into sheets by a combination of C—H...O and C—H...π(arene) hydrogen bonds. The two independent molecules of compound (IV) form two different centrosymmetric dimers, one built from inversion‐related pairs of C—H...O hydrogen bonds and the other from inversion‐related pairs of C—H...π(arene) hydrogen bonds. Comparisons are made with related compounds. 相似文献
2.
Jayashree Avvadukkam Narayana Badiadka Sarojini B. Kunhanna Madan S. Kumar 《Journal of heterocyclic chemistry》2021,58(3):724-736
A facile three-component reaction of aromatic aldehyde, 2,2-dimethyl-1,3-dioxane-4,6-dione, and 6-amino-1,3-dimethyluracil was developed for the first time using β-cyclodextrin (β-CD) as a macrocyclic host for aldehyde and an efficient catalyst that leads to a batch of novel pyrano[2,3-d:6,5-d′]dipyrimidines ( 4a-k ). The synthesis was accomplished with the aid of microwave irradiations in solvent-free conditions. The product obtained was in contrast to the previous report in which a similar reaction resulted in a mixture of benzylidenepyrimidine and bisaminopyrimidine analogs in the presence of triethylbenzylammonium chloride in an aqueous medium. The formation of the pyrano[2,3-d:6,5-d′]dipyrimidines may be in virtue of the property of β-CD to construct new C C and C X (where X = heteroatom) bonds. Reusability of the catalyst up to three runs without any noteworthy change in catalytic activity is one of the main features of the reaction. Other noteworthy features are good to excellent yields, eco-friendly procedure, non-column chromatographic purification, and mild conditions. 相似文献
3.
Mathew Mendalin Narayana Badiadka Sreekumar Naracham Veedu Vipin Kuttamath 《Mikrochimica acta》2004,144(4):291-295
A rapid and sensitive spectrophotometric method is described for the determination of trace amounts of cerium using Variamine Blue (VB) as a chromogenic reagent. The proposed method is based on the reaction of cerium with potassium iodide in acidic medium to liberate iodine, which oxidizes Variamine Blue to give a violet colored species with an absorption maximum at 560nm. Beers law was obeyed in the range 2–10µg mL–1 of cerium. The molar absorptivity and Sandells sensitivity are found to be 1.65×104L mol–1cm–1 and 8.48×10–3µgcm–2, respectively. The proposed method has been successfully applied to the determination of cerium in alloy and synthetic mixtures. 相似文献
4.
5.
Karanth N. Subbulakshmi Badiadka Narayana Hemmige S. Yathirajan Mehmet Akkurt
mer elik Cem Cüneyt Ersanl Christopher Glidewell 《Acta Crystallographica. Section C, Structural Chemistry》2015,71(8):742-751
Syntheses and structures are described for some alkylidene‐substituted dihydrooxazolones and dihydroimidazoles derived from simple acylglycines. A second, triclinic, polymorph of 4‐benzylidene‐2‐(4‐methylphenyl)‐1,3‐oxazol‐5(4H)‐one, C17H13NO2, (I), has been identified and the structure of 2‐methyl‐4‐[(thiophen‐2‐yl)methylidene]‐1,3‐oxazol‐5(4H)‐one, C9H7NO2S, (II), has been rerefined taking into account the orientational disorder of the thienyl group in each of the two independent molecules. The reactions of phenylhydrazine with 2‐phenyl‐4‐[(thiophen‐2‐yl)methylidene]‐1,3‐oxazol‐5(4H)‐one or 2‐(4‐methylphenyl)‐4‐[(thiophen‐2‐yl)methylidene]‐1,3‐oxazol‐5(4H)‐one yield, respectively, 3‐anilino‐2‐phenyl‐5‐[(thiophen‐2‐yl)methylidene]‐3,5‐dihydro‐4H‐imidazol‐4‐one, C10H15N3OS, (III), and 3‐anilino‐2‐(4‐methylphenyl)‐5‐[(thiophen‐2‐yl)methylidene]‐3,5‐dihydro‐4H‐imidazol‐4‐one, C21H17N3OS, (IV), which both exhibit orientational disorder in their thienyl groups. The reactions of 2‐phenyl‐4‐[(thiophen‐2‐yl)methylidene]‐1,3‐oxazol‐5(4H)‐one with hydrazine hydrate or with water yield, respectively, N‐[3‐hydrazinyl‐3‐oxo‐1‐(thiophen‐2‐yl)prop‐1‐en‐2‐yl]benzamide and 2‐(benzoylamino)‐3‐(thiophen‐2‐yl)prop‐2‐enoic acid, which in turn react, respectively, with thiophene‐2‐carbaldehyde to form 2‐phenyl‐5‐[(thiophen‐2‐yl)methylidene]‐3‐{[(E)‐(thiophen‐2‐yl)methylidene]amino}‐3,5‐dihydro‐4H‐imidazol‐4‐one, C19H13N3OS2, (V), which exhibits orientational disorder in only one of its thienyl groups, and with methanol to give methyl (2Z)‐2‐(benzoylamino)‐3‐(thiophen‐2‐yl)prop‐2‐enoate, C15H13NO3S, (VI). There are no direction‐specific intermolecular interactions in the crystal structure of the triclinic polymorph of (I), but the molecules of (II) are linked by two independent C—H...O hydrogen bonds to form C22(14) chains. Compounds (III) and (IV) both form centrosymmetric R22(10) dimers built from N—H...O hydrogen bonds, while compound (V) forms a centrosymmetric R22(10) dimer built from C—H...O hydrogen bonds. In the structure of compound (VI), a combination of N—H...O and C—H...π(arene) hydrogen bonds links the molecules into sheets. Comparisons are made with some similar compounds. 相似文献
6.
7.
Aletti S. Praveen Hemmige S. Yathirajan Manpreet Kaur Badiadka Narayana Eric C. Hosten Richard Betz Christopher Glidewell 《Acta Crystallographica. Section C, Structural Chemistry》2014,70(9):920-926
Four imidazo[2,1‐b][1,3,4]thiadiazoles containing a simply‐substituted 6‐aryl group have been synthesized by reaction of 2‐amino‐1,3,4‐thiadiazoles with bromoacetylarenes using microwave irradiation and brief reaction times. 6‐(2‐Chlorophenyl)imidazo[2,1‐b][1,3,4]thiadiazole, C10H6ClN3S, (I), 6‐(2‐chlorophenyl)‐2‐methylimidazo[2,1‐b][1,3,4]thiadiazole, C11H8ClN3S, (II), 6‐(3,4‐dichlorophenyl)imidazo[2,1‐b][1,3,4]thiadiazole, C10H5Cl2N3S, (III), and 6‐(4‐fluoro‐3‐methoxyphenyl)‐2‐methylimidazo[2,1‐b][1,3,4]thiadiazole, C12H10FN3OS, (IV), crystallize with Z′ values of 2, 1, 1 and 2 respectively. The molecular skeletons are all nearly planar and the dihedral angles between the imidazole and aryl rings are 1.51 (8) and 7.28 (8)° in (I), 9.65 (7)° in (II), 10.44 (8)° in (III), and 1.05 (8) and 7.21 (8)° in (IV). The molecules in (I) are linked by three independent C—H...N hydrogen bonds to form ribbons containing alternating R22(8) and R44(18) rings, and these ribbons are linked into a three‐dimensional array by three independent π‐stacking interactions. Both (II) and (III) contain centrosymmetric dimers formed by π‐stacking interactions but hydrogen bonds are absent, and the molecules of (IV) are linked into centrosymmetric R22(8) dimers by C—H...N hydrogen bonds. Comparisons are made with a number of related compounds. 相似文献
8.
Badiadka Narayana Mendalin Mathew Nekkarakalaya Gopalakrishna Bhat Naracham Veedu Sreekumar 《Mikrochimica acta》2003,141(3-4):175-178
This study describes a rapid and sensitive spectrophotometric method for the determination of trace amounts of selenium,
using starch and iodine as chromogenic reagents. The proposed method is based on the reaction of selenium with potassium iodide
in an acidic medium to liberate iodine. This reacts with starch to form a blue colored species with an absorption maximum
of 570 nm. Beer’s Law was obeyed in the range of 2–12 μg of selenium. The molar absorptivity and Sandell’s sensitivity were
found to be 1.40×104 L mol−1 cm−1 and 5.45×10−3 μg cm−2 respectively. The proposed method was successfully applied to determine selenium in a sample of natural water, polluted water,
soil sludge, biological samples and human hair.
Correspondence: Department of Studies in Chemistry, Managalore University, Mangalagangothri, Karnataka, India. e-mail: nbadiadka@yahoo.co.uk
Received August 2, 2002; accepted October 29, 2002 相似文献
9.
Badiadka Narayana Hemmige S. Yathirajan Ravindranath S. Rathore Christopher Glidewell 《Acta Crystallographica. Section C, Structural Chemistry》2016,72(9):664-669
4‐Antipyrine [4‐amino‐1,5‐dimethyl‐2‐phenyl‐1H‐pyrazol‐3(2H)‐one] and its derivatives exhibit a range of biological activities, including analgesic, antibacterial and anti‐inflammatory, and new examples are always of potential interest and value. 2‐(4‐Chlorophenyl)‐N‐(1,5‐dimethyl‐3‐oxo‐2‐phenyl‐2,3‐dihydro‐1H‐pyrazol‐4‐yl)acetamide, C19H18ClN3O2, (I), crystallizes with Z′ = 2 in the space group P, whereas its positional isomer 2‐(2‐chlorophenyl)‐N‐(1,5‐dimethyl‐3‐oxo‐2‐phenyl‐2,3‐dihydro‐1H‐pyrazol‐4‐yl)acetamide, (II), crystallizes with Z′ = 1 in the space group C2/c; the molecules of (II) are disordered over two sets of atomic sites having occupancies of 0.6020 (18) and 0.3980 (18). The two independent molecules of (I) adopt different molecular conformations, as do the two disorder components in (II), where the 2‐chlorophenyl substituents adopt different orientations. The molecules of (I) are linked by a combination of N—H…O and C—H…O hydrogen bonds to form centrosymmetric four‐molecule aggregates, while those of (II) are linked by the same types of hydrogen bonds forming sheets. The related compound N‐(1,5‐dimethyl‐3‐oxo‐2‐phenyl‐2,3‐dihydro‐1H‐pyrazol‐4‐yl)‐2‐(3‐methoxyphenyl)acetamide, C20H21N3O3, (III), is isomorphous with (I) but not strictly isostructural; again the two independent molecules adopt different molecular conformations, and the molecules are linked by N—H…O and C—H…O hydrogen bonds to form ribbons. Comparisons are made with some related structures, indicating that a hydrogen‐bonded R22(10) ring is the common structural motif. 相似文献
10.
Narachum V. Sreekumar Nellikalaya G. Bhat Badiadka Narayana Ronald A. Nazareth Prashant Hegde Busnur R. Manjunatha 《Mikrochimica acta》2003,141(1-2):29-33
A simple, rapid and accurate complexometric method is proposed for the determination of titanium(IV) where sodium potassium
tartrate or ascorbic acid were used as masking agents. In the presence of diverse metal ions, titanium is first complexed
with excess of EDTA and surplus EDTA is then titrated at pH 5–6 with zinc sulfate, xylenol orange being used as indicator.
An excess of 5% aqueous sodium potassium tartrate is then added to displace the complexed EDTA from the Ti-EDTA complex quantitatively,
which is titrated with zinc sulfate. Also, ascorbic acid may be used as the releasing agent. The methods work well in the
range 1–53 mg of Ti(IV) for sodium potassium tartrate with relative errors ± 0.28% and standard deviations ≤ 0.16 mg. For
ascorbic acid the range is 1.00–30.00 mg of Ti(IV) with relative errors of ± 0.40% and standard deviations of ≤ 0.05 mg
Received October 9, 2001; accepted August 2, 2002 相似文献