Preparations, sulphinate coordination, and thermal decomposition of some bismuth triarenesulphinates

1972 ◽  
Vol 25 (10) ◽  
pp. 2107 ◽  
Author(s):  
GB Deacon ◽  
GD Fallon

Bismuth triarenesulphinates, Bi(02SR)3 [R = Ph, p-MeC6H4, p-ClC6H4, 2,4,6-(Me2CH)3C6H2, and p-MeCONHC6H4], have been prepared by reaction of bismuth triacetate with the appropriate arenesulphinio acids in glacial acetic acid, and the first two compounds have also been obtained by reaction of triphenyl-bismuth with the appropriate mercuric arenesulphinates. The sulphur-oxygen stretching frequencies of the bismuth sulphinates are indicative of O-sulphinate coordination, and the compounds are considered to be polymeric with bridging O-sulphinate groups and six-coordinate bismuth. Thermal decomposition of Bi(O2SR)3 (R = Ph, p-MeC6H4, or p-CIC6H4) under vacuum gave the corresponding triarylbismuth compounds and sulphur dioxide, the preparation of tri-p-chlorophenylbismuth being accompanied by formation of di-p-chlorophenyl sulphone and S-p-chlorophenyl p-chlorobenzenethiosulphonate. Pyrolysis of the other triarenesulphinates did not yield organobismuth compounds.

1987 ◽  
Vol 33 (2) ◽  
pp. 289-292 ◽  
Author(s):  
G Csako

Abstract All free-sulfhydryl compounds tested produced false-positive reactions in the Legal test for ketones. The color developed in the ketone pad of urine dipsticks [N-Multistix SG, Multistix 10 SG (Ames), and Chemstrip 9 (Boehringer-Mannheim)] was misinterpreted for ketone bodies, both by visual and automated reading. In contrast to the reaction with true ketones, a drop of glacial acetic acid added onto the ketone pad of dipsticks discharged the false-positive red color. A red-violet also developed instantly with free -SH compounds in the Acetest tablet assay (Ames), but quickly faded. In general, the presence of acidic groups such as -COOH and -SO3H in the structure appeared to increase the nitroprusside reactivity of free -SH compounds, whereas the presence of a -NH2 group appeared to decrease it. Currently, false-positive ketone reactions ascribable to a free -SH group are most likely to be seen for urine containing mesna. The false-positive test for ketones caused by free -SH compounds can be recognized and ruled out by proper procedures. On the other hand, this chromogenic reaction with free thiols might be used for monitoring urinary excretion of mesna.


1980 ◽  
Vol 35 (10) ◽  
pp. 1310-1312 ◽  
Author(s):  
El-Sayed Afsah ◽  
Fathy A. Amer ◽  
Mohamed A. Metwally ◽  
Mohamed T. El-Zimaity

Abstract Treatment of diethyl 1,4-cyclohexanedione-2,5-dicarboxylate (1) with hydrazine hydrate in glacial acetic acid afforded the diazobicycloocatdienedicarboxylate (2) and the azine (3). On the other hand, condensation of 1 with benzenesulphonylhydrazide in ethanolic solution gave the indazole derivative (4). Interaction of 1 with urea or hydroxyl-amine afforded the tetrahydropyrimidoquinazolinone (5) and the tetrahydrobenzodi-isoxazolone (6), respectively. Treatment of 1 with aniline gave the mono-anil (7) which, when subjected to Japp-Klingemann reaction with p-anisidine gave the dihydrazonoanil (8) and their condensation with benzidine in acetic acid gave the hydrazonoketoester (9). On the other hand condensation of 7 with hydrazine hydrate in ethanolic solution afforded the azobis (5-anilinoterephthalate) (10) and the hexahydrobenzodipyrazolone (11).


1969 ◽  
Vol 22 (3) ◽  
pp. 549 ◽  
Author(s):  
GB Deacon ◽  
PW Felder

The arylmercuric arenesulphinates, PhHg(SO2Ph), p-MeC6H4Hg(SO2-p-MeC6H4), PhHg(SO2-p-MeC6H4), p-MeC6H4Hg(SO2Ph), and C6F5Hg(SO2Ph), have been prepared by reaction of mercuric benzenesulphinate or p- toluenesulphinate with the appropriate diarylmercury compound in chloroform or methanol, and the first three compounds have also been obtained by reaction of liquid sulphur dioxide with diphenylmercury, di-p-tolylmercury, or phenyl-p-tolylmercury. Linkage isomers of phenylmercuric benzenesulphinate have been prepared. Isomer A, obtained from chloroform-pentane, is considered to be a monomeric O-sulphinato complex, and isomer B, obtained from cold acetone, methyl ethyI ketone, or methanol, to be an S-sulphinato complex. The isomers are readily interconverted. In chloroform, deuterochloroform, and acetone, at room temperature, only the O-sulphinato complex can be detected. The other arylmercuric arenesulphinates have the same structure as isomer A. Linkage isomers could not be isolated for these derivatives. However, there is evidence that p-MeC6H4Hg(SO2Ph) slowly isomerizes in the solid state to give the corresponding S-sulphinato complex. Thermal decomposition of PhHg-(SO2Ph) (both isomers), p-MeC6H4Hg(SO2-p-MeC6H4), PhHg(SO2-p-MeC6H4), and p-MeC8H4Hg(SO2Ph) gives sulphur dioxide and the corresponding diarylmercurycompound.


2012 ◽  
Vol 47 (No. 1) ◽  
pp. 1-4 ◽  
Author(s):  
V. Rada ◽  
J. Petr

TPY agar supplemented with mupirocin (100 mg/liter) and glacial acetic acid (1 ml/liter) was effective in the enumeration of bifidobacteria in animal (11 species) fecal or intestinal samples. On the other hand, less than 50% of isolates from pig feces were identified as Bifidobacterium sp. using this medium. Subsequently TPY agar modified by the addition of mupirocin (100 mg/liter), glacial acetic acid (1 ml/liter), and colistin (25 mg/liter) was developed for the enumeration of bifidobacteria in pig feces. The results suggest that the bifidobacteria selective media should be chosen in respect of the animal species origin of the samples tested.


1957 ◽  
Vol 35 (12) ◽  
pp. 1423-1433 ◽  
Author(s):  
Paul E. Gagnon ◽  
Karl F. Keirstead ◽  
Brian T. Newbold

The properties of chlorotrihydroxydihydrophenazine were thoroughly investigated. Oxidations with sodium perborate or hydrogen peroxide in glacial acetic acid gave chloro-trihydroxyphenazine-5,10-dioxide. Methylation gave a monomethyl derivative and acetylation yielded mono-, di-, and tri-acetyl derivatives. Benzoylation gave a tetrabenzoyl compound. Bromination gave a monobromo derivative. Nitrosation produced a mononitroso and nitration a mononitro compound. Degradation by zinc dust distillation and thermal decomposition yielded phenazine. Molecular weight and absorption spectra determinations supported the chemical evidence that the compound was 1-chloro-2(or 3),6,8-trihydroxydihydrophenazine. 1,4,9-Trichloro-2(or 3),6,8-trihydroxydihydrophenazine, 1,4,9-trichloro-2(or 3, or 8),6-dihy-droxydihydrophenazine, and 1-bromo-2(or 3),6,8-trihydroxydihydrophenazine were similarly identified.


Author(s):  
Alok Jain ◽  
Shailendra Patil ◽  
Asmita Gajbhiye

Aryl semicarbazide derivatives are reported to possess anticonvulsant activity. On the other hand unsubstituted and small substituents (less than 3 carbon atom) containing cyclohexanones prevented both pentylenetetrazole and MES induced seizures. Similarly cycloheptanone fused with benzodiazepine and furan produced anticonvulsant compounds. Therefore looking into the above facts in the present study, we have synthesized 12 derivatives of 1-cyclohexylidine/cycloheptylidine-4-substitued semicarbazide derivatives and screened them for anticonvulsant activity. The synthesis of compounds was achieved as follows: The various para substituted (H, CH3, F,Cl,Br, I) anilines were converted to aryl ureas by reacting with sodium cyanate in the presence of glacial acetic acid. These aryl ureas and aryl semicarbazides were synthesized by allowing them to react with hydrazine hydrate. Finally the aryl semicarbazides were condensed with cyclohexanone/ cycloheptanone in the presence of sodium acetate to give title compounds. All the synthesized compounds were evaluated for anticonvulsant activity by MES method using carbamazepine as standard and it was observed that all the compounds possess anticonvulsant activity comparable to carbamazepine. Carbamazepine had shown the abolition in the hind limb extensor tonic convulsion after 2 sec. whereas few compounds i.e. 1-cyclohexylidine-4-(4-fluorophenyl) semicarbazide, 1-cycloheptylidine-4-(4- fluorophenyl) semi-carbazide and 1-cycloheptylidine-4-phenylsemicarbazide were more active than standard. Overall it was found that cycloheptyl containing compounds were more active than cyclohexyl containing compounds. The unsubstitued compounds were more active than halo derivatives i.e. electron withdrawing groups, and halo compounds were more active than methyl derivatives i.e. electron donating group (CH3). The order of activity for cyclohexanone and cycloheptanone derivatives is as follows: H >F >Cl >Br >I >CH3. Among the halo derivatives, the activity decreased with increasing molecular weight of halo substituents.


2008 ◽  
Vol 59 (1) ◽  
pp. 41-44
Author(s):  
Maria-Daniela Sofei ◽  
Maria Ilici ◽  
Valentin Badea ◽  
Carol Csunderlik ◽  
Vasile-Nicolae Bercean

The synthesis of 1H-3-aryl-7-ethoxycarbonyl-6-methyl-pyrazolo[5,1-c][1,2,4]triazoles (2) was carried out by cyclization of 1H-5-arylidenehydrazino-4-ethoxycarbonyl-3-methyl-pyrazoles (1) in the presence of bromine using glacial acetic acid as solvent and sodium acetate as base. The new nine obtained compounds were characterized by IR and NMR spectroscopy and mass spectrometry.


1979 ◽  
Vol 44 (8) ◽  
pp. 2330-2337 ◽  
Author(s):  
Jindřiška Maternová ◽  
Anastas A. Andreev ◽  
Dimitrii M. Shopov ◽  
Karel Setínek

It was found spectroscopically that cobalt(II) acetate dissolved in glacial acetic acid forms the octahedral complex [Co(OAc)2(HOAc)4] which in the presence of bromide ions gives the octahedral [Co(OAc)Br(HOAc)4] and tetrahedral bromo(acetate)cobalt(II) complexes with the higher number of Br- ions. When attached to an organic polymer cobalt(II) ions are bonded in the form of octahedral [Co(H2O)6]2+ cations which form with acetic acid similar complexes as in homogeneous phase and are able to coordinate one bromide ion. Drying the copolymer possessing octahedral hexaaquocobalt(II) cations leads to tetrahedral aquocomplexes which are solvated by gaseous acetic acid and converted into the acetate complexes with the liquid acid. The latter contain the acid in the inner coordination sphere and have tetrahedral symmetry.


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