Synthesis of Hexahydroindazole, Tetrahydro-[pyrimidoquinazolinone, benzodiisoxazolone] Derivatives and Anils from Diethyl 1,4-Cyclohexanedione-2,5-dicarboxylate

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).

1976 ◽  
Vol 31 (7) ◽  
pp. 989-992 ◽  
Author(s):  
Mohamed Mohamed Mohamed Sallam ◽  
Mohamed Helmy Elnagdi ◽  
Daizy Hanna Fleita ◽  
Eric Hartmann

Diethyl phenylthiocarbamoylmalonate (2) reacts with β-cyanoethylhydrazin (1) to yield ethyl 3-anilino-2-pyrazolin-5-one (3) via decyanoethylation of the reaction intermediates.Whereas 2 reacts with hydrazine hydrate in refluxing ethanol to yield a mixture of 3-anilino-2-pyrazolin-5-one (4) and the hydrazide (5), the diethyl ester (6) is formed on treatment of 2 with the same reagent in a cooled ethanolic solution. On the other hand, 2 reacts with hydrazine hydrate in the absence of a solvent to yield the carboxylic acid (7).Benzoylacetonitrile reacts with phenylisothiocyanate to yield the thioanilide (8). The latter compound neither reacts with hydrazine hydrate not β-cyanoethylhydrazine.


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.


2013 ◽  
Vol 9 ◽  
pp. 8-14 ◽  
Author(s):  
Yan Sun ◽  
Jing Sun ◽  
Chao-Guo Yan

A fast and convenient protocol for the synthesis of novel spiro[dihydropyridine-oxindole] derivatives in satisfactory yields was developed by the three-component reactions of arylamine, isatin and cyclopentane-1,3-dione in acetic acid at room temperature. On the other hand the condensation of isatin with two equivalents of cyclopentane-1,3-dione gave 3,3-bis(2-hydroxy-5-oxo-cyclopent-1-enyl)oxindole in high yields. The reaction mechanism and substrate scope of this novel reaction is briefly discussed.


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.


1977 ◽  
Vol 32 (6) ◽  
pp. 701-704 ◽  
Author(s):  
Gert Kollenz ◽  
Erich Ziegler ◽  
Walter Ott ◽  
Gert Kriwetz

4-Benzoyl-5-phenyl-2,3-dihydrofuran-2,3-dione (1) reacts with aldehydes or ketones via the acylketene-intermediate (2) yielding the 1,3-dioxin-4-ones (3). The aldehyde derivatives (3 a-e) can be converted into the anilino-chalcone (5) or the anilino acrylic acid (6) by treating with aniline at 20 °C. 6 and diazomethane combine to the acrylic acid methyl ester (7), which by heating (200 °C) is cyclisized to the quinolin-4-ole (8). On the other hand, the keto derivatives 3f-h and aniline give the dibenzoyl acetic acid anilide (9).


1966 ◽  
Vol 44 (17) ◽  
pp. 2009-2014 ◽  
Author(s):  
R. T. Coutts ◽  
J. B. Edwards

4-(2-Nitrobenzylidene)-2-pyrazolin-5-ones (I) were best prepared by heating o-nitrobenzaldehyde and 2-pyrazolin-5-ones in acetic anhydride containing fused sodium acetate (cf. Erlenmeyer azlactone synthesis). Pyrazolones of type I were reductively cyclized with cyclohexene and palladium–charcoal, and gave 3a,4,9,9a-tetrahydro-9-hydroxy-1H-pyrazolo-[3,4-b]quinolines (II) which, as expected, were amphoteric compounds. Of the three other methods of reduction used in this study, two (zinc and acetic acid; sodium borohydride and palladium–charcoal) were capable of producing pyrazoloquinolines, but were less reliable. The other method employed (hydrazine hydrate and palladium–charcoal) caused degradation of the pyrazolone molecule in the two cases examined, and in both, bis(2-aminobenzylidene) hydrazine (V) was the reduction product isolated.


1979 ◽  
Vol 34 (3) ◽  
pp. 507-510 ◽  
Author(s):  
Nazmi A. Kassab ◽  
Sanaa O. Abd Allah ◽  
Said A. Elbahaii

Abstract The 5-arylhydrazono derivatives of rhodanine and isorhodanine were subjected to the action of hydrazine hydrate to afford the arylhydrazonomercaptomethyl-triazolinones (3) and -triazolinthiones (3) respectively. Treatment of 1 with benzylamine afforded thioxalic acid dibenzylamide (5). On the other hand treatment of 2 with the same reagent afforded the corresponding benzylimino derivatives (6).Alkylation of 1 and 2 with ethyl bromoacetate and chloroacetamide yielded the corresponding S-alkyl derivatives (7) and (8), respectively.


2019 ◽  
Vol 7 (1) ◽  
Author(s):  
Sarka Msallamova ◽  
Milan Kouril ◽  
Kristyna Charlotte Strachotova ◽  
Jan Stoulil ◽  
Kateryna Popova ◽  
...  

Abstract Historical museums and depositories contain collections with a number of lead objects or historical documents with lead seals. Lead is a metal which has good corrosion resistance under atmospheric conditions. On the other hand, lead corrodes in an activity in an environment which contains volatile organic compounds (mainly acetic acid and formic acid). In a depository environment, sources of volatile compounds can be the historical documents themselves, wood, plastics (those made from cellulose acetate), polyvinyl acetate adhesives, varnishes, oil or emulsion paints, etc. The aim of this work was to compare the efficiency of commercial adsorbents (activated carbon, activated alumina, zeolite, and bentonite) in the acetic acid vapours. The lead corrosion rates were determined by using lead resistometric probes. Activated alumina and activated carbon were found to be the most effective adsorbents of acetic acid vapours. On the other hand, the available zeolite had the worst sorption ability compared with the other tested substances.


2016 ◽  
Vol 8 (1) ◽  
pp. 1464-1471 ◽  
Author(s):  
Rafid H. Al-Asadi ◽  
Tarik A. Fahad ◽  
Bahjat A. Saeed ◽  
Wasfi A. Al-Masoudi

New tellurated schiff bases were synthesized by the reaction of the corresponding mercurated Schiff  bases compounds A1-A3 with tellurium tetrabromide in 1:1 mole ratio and  that  gave organyltellurium tribromides  A4-A6.  On the other hand, when mercurated schiff bases and tellurium tetrabromide brought  together in 2:1 mole ratio gave diorganyltellurium dibromides compounds A10-A12 followed by reduction with hydrazine hydrate gave new diorganyl tellurides A13-A15.  Reduction of compounds A4-A6 by  hydrazine hydrate gave new ditellurides A7-A9.  All compounds were characterized by elemental analysis, IR, 1H , 13C NMR, HSQC-NMR and mass spectra.  Invitro anti-tumor bioactivity of some compounds were tested. 


Author(s):  
Gilbert Y. Kennedy

Munro Fox (1926, Addendum, p. 219) described a method of preparation of chlorocruoroporphyrin from the blood of the marine polychaete worm Spirographis. This was based upon the very troublesome method of Nencki & Zaleski (1900), which is time-consuming and wasteful. Furthermore, Spirographis is not easily obtainable in this country. Lemberg & Parker (1952) started with protoporphyrin, and by careful oxidation with potassium permanganate in acetone obtained a solution which gaVe mixed crystals of chlorocruoroporphyrin and diformyldeuteroporphyrin esters. Purification was by fractional chromatography. The procedure to be described here is simple and rapid, and could easily be carried out in one day by a biologist requiring a small sample of the porphyrin. The two methods mentioned above would not come into this category.This work was done at the Plymouth Laboratory, and I am very grateful to Mr T. R. Tozer of that laboratory for so kindly obtaining the animals for me and extracting the blood.The polychaete worms Myxicola infundibulum, Sabella pavonina and Branchiomma vesiculosum are all readily obtained from the muddy shores of the Salcombe estuary, especially on the Salstone. Blood was taken directly from the vessels of about 100 assorted worms by syringe, and squirted as it was removed from the worms into a mixture of peroxide-free ether (3 parts) and ‘Analar’ glacial acetic acid (1 part). After all the blood had been added, the mixture was well shaken and allowed to stand in the ice-chest for 30 min. The acetic acid was then washed out with distilled water, the first few washings containing a little sodium acetate to avoid washing out of the pigment, and the remaining solution of chlorocruorohaematin dried roughly by filtering through ether-soaked paper into a distilling flask and evaporated to dryness. 100 ml. of a 50% solution of hydrazine hydrate in glacial acetic acid were then added, and the mixture heated on a water-bath at 90° C. for 10 min.


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