Carbonyl-Containing Spirodihydrofurans in Reactions with Ammonium Acetate and Hydrazine Hydrate.

ChemInform ◽  
2006 ◽  
Vol 37 (32) ◽  
Author(s):  
O. V. Fedotova ◽  
M. I. Skuratova ◽  
P. V. Reshetov ◽  
M. A. Panov
2003 ◽  
Vol 56 (12) ◽  
pp. 1219 ◽  
Author(s):  
Leslie W. Deady ◽  
Clare L. Smith

Acetophenones (H, o-, m-, p-Cl, o-aza) react with aminoanthraquinone in pyridine containing solid sodium hydroxide to form 6-(arylcarbonyl)methyl-2-aryl-7H-naphtho[1,2,3-de]quinolin-7-ones (with the 4-(arylcarbonyl)methyl isomer as minor product). Preformed 7H-benzo[e]perimidin-7-one with acetophenone underwent the second part of this process, i.e. nucleophilic substitution to form 6-phenacyl-7H-benzo-[e]perimidin-7-one. Further reactions are described, including cyclization with ammonium acetate/acetic acid to 2,7-diphenyl-1,6-diazabenzo[e]pyrene and 7-phenyl-1,3,8-triazabenzo[e]pyrene, respectively, and with hydrazine hydrate to 3,8-diphenyl-4H-[1,2]diazepino[3,4-4′,3′ : 4,5-f]naphtho[1,2,3-de]quinoline and 3-phenyl-4H-benzo[e][1,2]diazepino[3,4,5-gh]perimidine.


2005 ◽  
Vol 41 (12) ◽  
pp. 1480-1483 ◽  
Author(s):  
O. V. Fedotova ◽  
M. I. Skuratova ◽  
P. V. Reshetov ◽  
M. A. Panov

2007 ◽  
Vol 2007 (9) ◽  
pp. 541-544 ◽  
Author(s):  
Mahmoud R. Mahmoud ◽  
Eman A.A. El-Bordany ◽  
Naglaa F. Hassan ◽  
Fatma S.M. Abu El-Azm

2-undecyl-4H-3,1-benzoxazin-4-one (2) was prepared and reacted with primary and secondary amines affording compounds 3–7, while with hydrazine hydrate it gave the quinazolinone derivative 8. The reaction of 8 with 3,4,5-trimethoxybenzaldehyde followed by thioglycollic acid yielded 9 and 10, respectively. Acylation of 8 using cinnamoyl chloride gave 11. Furthermore, treatment of 2 with hydrazine derivatives provided 12 and 13. Fusion of 2 with ammonium acetate gave the quinazolinone derivative 14 which upon treatment with ethyl chloroacetate yielded the ester 15. The hydrazide 17 was obtained from hydrazinolysis of the ester 15.


1998 ◽  
Vol 76 (4) ◽  
pp. 469-476 ◽  
Author(s):  
M ZA Badr ◽  
A A Geies ◽  
M S Abbady ◽  
A A Dahy

3-Cyano-4-(p-tolyl)pyrido[3,2-c]cinnolin-2(1H) thione 3 was reacted with α -halo ketones, esters, or amides to give the intermediates, S-alkylated products 5b-h, respectively, which underwent intramolecular ring closure reactions with ethanolic sodium ethoxide to give thienopyridocinnolines 6a-h. Pyrimidothienopyridocinnolines 9 and 11 were obtained by treatment of oxazino compound 8 with hydrazine hydrate and ammonium acetate. Treatment of hydrazino derivative 13 with acetylacetone, triethylorthoformate, carbon disulphide, ethyl chloroformate, and acetic anhydride afforded triazolopyrimidothienopyridocinnolines 14-16, 18, and 21, while with nitrous acid the corresponding tetrazolo compound 19 was produced.Key words: thienopyridocinnolines; their pyrimido, triazolopyrimido, and heteroannelated systems.


Author(s):  
A.-M. Ladhoff ◽  
B.J. Thiele ◽  
Ch. Coutelle ◽  
S. Rosenthal

The suggested precursor-product relationship between the nuclear pre-mRNA and the cytoplasmic mRNA has created increased interest also in the structure of these RNA species. Previously we have been published electron micrographs of individual pre-mRNA molecules from erythroid cells. An intersting observation was the appearance of a contour, probably corresponding to higher ordered structures, on one end of 10 % of the pre-mRNA molecules from erythroid rabbit bone marrow cells (Fig. 1A). A virtual similar contour was observed in molecules of 9S globin mRNA from rabbit reticulocytes (Fig. 1B). A structural transformation in a linear contour occurs if the RNA is heated for 10 min to 90°C in the presence of 80 % formamide. This structural transformation is reversible when the denatured RNA is precipitated and redissolved in 0.2 M ammonium acetate.


Author(s):  
N. H. Sarkar ◽  
Dan H. Moore

Mouse mammary tumor virus (MTV) is believed to contain about 0.8% single stranded ribonucleic acid (RNA). This value of RNA content was estimated on a dry weight basis. The subject of this report is an attempt to visualize the RNA molecules of MTV particles.MTV particles were isolated from RIII mouse (tumor incidence approximately 80%) milk according to the method described by Lyons and Moore. Purified virions from 5 ml of milk were finally suspended in 0.2 ml of PBS, pH 7.4 and was mixed with an equal volume of pronase (5 mg/ml). This mixture was incubated at 37°C for an hour. RNA was extracted three times using freshly prepared cold phenol. It was then treated three times with cold ethyl ether to remove any trace of phenol. The RNA thus extracted was divided into two parts. One part was diluted four fold with 8M urea to avoid aggregation of the molecules. The other part was left untreated. Both samples were then mixed with an equal volume of 1M ammonium acetate, adjusted to pH 8.0 with NH3 containing chymotrypsin at a concentration of 0.01%.


Author(s):  
E.T. O’Toole ◽  
G.P. Wray ◽  
J.R. Kremer ◽  
J.R. Mcintosh

Ultrarapid freezing and cryomicroscopy of frozen hydrated material makes it possible to visualize samples that have never been exposed to chemical fixatives, dehydration, or stains. In principle, freezing and cryoimaging methods avoid artifacts associated with chemical fixation and processing and allow one to visualize the specimen in a condition that is close to its native state. Here we describe a way to use a high voltage electron microscope (HVEM) for the cryoimaging of frozen hydrated PTK1 cells.PTK1 cells were cultured on formvar-coated, carbon stabilized gold grids. After three days in culture, the grids were removed from the culture medium and blotted in a humidity chamber at 35° C. In some instances, the grids were rinsed briefly in 0.16 M ammonium acetate buffer (pH 7.2) prior to blotting. After blotting, the grids were transferred to a plunging apparatus and plunged into liquid ethane held directly above its freezing point. The plunging apparatus consists of a vertical slide rail that guides the fall of a mounted pair of forceps that clamp the specimen. The forceps are surrounded by a plexiglass humidity chamber mounted over a dewar of liquid nitrogen containing an ethane chamber. After freezing, the samples were transferred to liquid nitrogen and viewed in a JEOL JEM 1000 equipped with a top entry cold stage designed and built by Mr. George Wray (Univ. Colorado). The samples were routinely exposed to electron doses of 1 e/Å2/sec, and viewed at a temperature of −150° C. A GATAN video system was used to enhance contrast and to estimate the correct amount of underfocus needed to obtain phase contrast at various magnifications. Low dose micrographs were taken using two second exposures of Kodak 4463 film. The state of the solid water in the specimen was determined by diffraction using a 30/μm field limiting aperture and a camera length of 1 meter.


2018 ◽  
Vol 21 (4) ◽  
pp. 271-280 ◽  
Author(s):  
Mohammad A. Ghasemzadeh ◽  
Mohammad H. Abdollahi-Basir ◽  
Zahra Elyasi

Aim and Objective: The multi-component condensation of benzil, primary amines, ammonium acetate and various aldehydes was efficiently catalyzed using cobalt oxide nanoparticles under ultrasonic irradiation. This approach describes an effective and facile method for the synthesis of some novel 1,2,4,5-tetrasubstituted imidazole derivatives with several advantages such as high yields and short reaction times and reusability of the catalyst. Moreover, the prepared heterocyclic compounds showed high antibacterial activity against some pathogenic strains. Materials and Method: The facile and efficient approaches for the preparation of Co3O4 nanoparticles were carried out by one step method. The synthesized heterogeneous nanocatalyst was characterized by spectroscopic analysis including EDX, FE-SEM, VSM, XRD and FT-IR analysis. The as-synthesized cobalt oxide nanoparticles showed paramagnetic behaviour in magnetic field. In addition, the catalytic influence of the nanocatalyst was examined in the one-pot reaction of primary amines, benzil, ammonium acetate and diverse aromatic aldehydes under ultrasonic irradiation. All of the 1,2,4,5-tetrasubstituted imidazoles were investigated and checked with m.p., 1H NMR, 13C NMR and FT-IR spectroscopy techniques. The antibacterial properties of the heterocycles were evaluated in vitro by the disk diffusion against pathogenic strains such as Escherichia coli (EC), Bacillus subtillis (BS), Staphylococcus aureus (SA), Salmonellatyphi (ST) and Shigella dysentrae (SD) species. Results: In this research cobalt oxide nanostructure was used as a robust and green catalyst in the some novel imidazoles. The average particle size measured from the FE-SEM image is found to be 20-30 nm which confirmed to the obtained results from XRD pattern. Various electron-donating and electron-withdrawing aryl aldehydes were efficiently reacted in the presence of Co3O4 nanoparticles. The role of the catalyst as a Lewis acid is promoting the reactions with the increase in the electrophilicity of the carbonyl and double band groups. To investigate the reusability of the catalyst, the model study was repeated using recovered cobalt oxide nanoparticles. The results showed that the nanocatalyst could be reused for five times with a minimal loss of its activity. Conclusion: We have developed an efficient and environmentally friendly method for the synthesis of some tetrasubstituted imidazoles via three-component reaction of benzil, primary amines, ammonium acetate and various aldehydes using Co3O4 NPs. The present approach suggests different benefits such as: excellent yields, short reaction times, simple workup procedure and recyclability of the magnetic nanocatalyst. The prepared 1,2,4,5-tetrasubstituted imidazoles revealed high antibacterial activities and can be useful in many biomedical applications.


Author(s):  
Shixing Zhu ◽  
Jiayuan Zhang ◽  
Zhihua Lv ◽  
Mingming Yu

Background: Apigenin, a natural plant flavone, has been shown to possess a variety of biological properties. Objective: In this report, a highly selective and sensitive LC-MS/MS method was developed and validated for the determination of apigenin in rat plasma. Methods: Analysts were separated on the HSS T3 column (1.8 μm 2.1×100 mm) using acetonitrile and 0.1% formic acid in 2 mM ammonium acetate buffer at a supply rate of 0.200 mL/min as eluent in gradient model. Results: Plasma samples were treated by protein precipitation using acetonitrile for the recovery ranging from 86.5% to 90.1% for apigenin. The calibration curves followed linearity in the concentration range of 0.50-500 ng/mL. The inter-day and intra-day precisions at different QC levels within 13.1% and the accuracies ranged from -10.6% to 8.6%. Conclusion: The assay has been successfully applied to the pharmacokinetic study of apigenin in rats.


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